Month: July 2021

Adding a certain compound to certain chemical reactions, such as: 84851-56-9, Methyl 4-(1-hydroxyethyl)benzoate, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, category: alcohols-buliding-blocks, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

EXAMPLE 3 A solution consisting of 3.6 g (0.02 mol) of V-1 obtained in Example 1 and 30 ml of dimethylformamide was cooled to 10 C., then added with 0.62 g (0.026 mol) of sodium hydride and kept at 30-35 C. for one hour. The mixture was further added with 7.69 g (0.03 mol) of n-hexyl tosylate at 20-25 C. and reacted at 40-50 C. for 5 hours. The reaction mixture was treated according to Example 1 to obtain 4.60 g (92% yield) of (+)-methyl 4-(1-hexyloxyethyl)benzoate (VII-3). ([alpha]D20 =+60.6 (c=1, CHCl3), nD20 =1.4922).

The synthetic route of 84851-56-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Sumitomo Chemical Company, Limited; US5019298; (1991); A;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 3391-86-4, name is Oct-1-en-3-ol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 3391-86-4

To estimate the oxidoreductase activity toward 5, crude enzyme soln. (100 muL) prepared as described in Section 4.4. was mixed with 10 mgmL-1 5 (10 muL) suspended in 0.2% Tween 20, and incubated at 27 C for 5 min in 50 mM sodium phosphate (pH 7.0) with or without 5 mM NADH or NADPH. After the reaction, the C8 compounds were extracted with 1 mL of MTBE containing nonanyl acetate (1 mugmL-1), and quantitatively analyzed using GC-MS essentially as described in Section 4.4 but with the modified column condition [40 C (5 min) to 200 C (2 min) at 8 Cmin-1 with He as a carrier gas at 26.7 cms-1].

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 3391-86-4, Oct-1-en-3-ol.

Reference:
Article; Kihara, Hirotomo; Tanaka, Maya; Yamato, Katsuyuki T.; Horibata, Akira; Yamada, Atsushi; Kita, Sayaka; Ishizaki, Kimitsune; Kajikawa, Masataka; Fukuzawa, Hideya; Kohchi, Takayuki; Akakabe, Yoshihiko; Matsui, Kenji; Phytochemistry; vol. 107; (2014); p. 42 – 49;,
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Electric Literature of 13330-96-6, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.13330-96-6, name is 4-(Dimethylamino)butan-1-ol, molecular formula is C6H15NO, molecular weight is 117.19, as common compound, the synthetic route is as follows.

To a solution of 4-nitrophenyl(6Z,9Z,26Z,29Z)-pentatriaconta-6,9,26,29-tetraen-18-yl carbonate (0.12 g, 0.18 mmol) obtained in Reference Example 5, 4-dimethylamino-1-butanol (0.22 g, 1.8 mmol), and diisopropylethylamine (0.10 g, 0.72 mmol) in dichloromethane (10 mL), 4-dimethylaminopyridine (0.09 g, 0.72 mmol) was added, and the mixture was reacted overnight at room temperature. After water treatment, the reaction mixture was subjected to extraction with dichloromethane, and the obtained organic layer was dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was then subjected to silica gel column chromatography to obtain the compound of interest as a colorless liquid (30 mg, 26%). 1H-NMR (400 MHz, CDCl3) delta: 0.89 (6H, t, J = 6.6 Hz), 1.21 – 1.42 (34H, m), 1.47 – 1.64 (6H, m), 1.71 (2H, tt, J = 6.6, 7.4 Hz), 1.99 – 2.09 (8H, m), 2.21 (6H, s), 2.27 (2H, t, J = 7.4 Hz), 2.77 (4H, t, J = 6.6 Hz), 4.14 (2H, t, J = 6.6 Hz), 4.63 – 4.72 (1H, m), 5.28 – 5.43 (8H, m). MS (ESI+) m/z 644 [M+H]+ HRMS (ESI+) m/z 644.6008 (2.6 mDa).

Statistics shows that 13330-96-6 is playing an increasingly important role. we look forward to future research findings about 4-(Dimethylamino)butan-1-ol.

Reference:
Patent; Daiichi Sankyo Company, Limited; KOIZUMI, Makoto; ONISHI, Yoshiyuki; NIWA, Takako; TAMURA, Masakazu; KASUYA, Yuji; (152 pag.)EP3020701; (2016); A1;,
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Synthetic Route of 5339-85-5, In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 5339-85-5 as follows.

COMPARATIVE EXAMPLE 8 The procedures of Example 13 were repeated except that 0.1 g of “CDT-60” was used without K2 CO3. The conversion of 2-(o-aminophenyl)ethanol was 28.6% and the yield of indole was 24.3%.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,5339-85-5, its application will become more common.

Reference:
Patent; Research Association for Utilization of Light Oil; US4757152; (1988); A;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 50595-15-8, name is tert-Butyl 2-hydroxyacetate. This compound has unique chemical properties. The synthetic route is as follows. Safety of tert-Butyl 2-hydroxyacetate

To a solution of Compound 37A (200 mg, 0.28 mmol) and DIAD (60 mg, 0.30 mmol) in THF (0.5 mL) was added a solution of triphenylphospine (78 mg, 0.30 mmol) and t-butyl-2-hydroxy acetate in THF (0.5 mL) dropwise. The resulting mixture was stirred for 18 hours and concentrated in vacuo. The residue was purified by silica gel chromatography (0 – 100 % EtOAc/Hexanes) to afford Compound 38A (170 mg, 75 %). S)-2-(( -(2-(4-(3-chloro-2-methyl-N-(l-(3-(3-methylpyridin-4-yl)phenyl)ethyl) phenylsulfonamido)butanamido)ethyl)sulfamoyl)amino)acetic acid (Compound 38) Compound 38A (170 mg, 0.21 mmol) was dissolved in 4 N HC1 (dioxane, 6 mL) and stirred for 2 hours. The mixture was partioned between EtOAc and water. The organic layers were concentrated in vacuo and the residue was purified by reverse phase chromatography (5-100% water/ AcN 0.25 % formic acid) to afford Compound 38 as the formate salt (41 mg, 29 %). LCMS (method A): m/z 666.4/668.4 (M+H)+. lH NMR (CDC13) delta 12.66 (bs, IH), 8.44 (bs, IH), 8.39 (d, IH), 7.85 (d, IH), 7.70 (t, IH), 7.65 (d, IH), 7.37 (q, 2H), 7.29-7.23 (m, 2H), 7.12 (t, IH), 7.07 (d, IH), 7.01 (s, IH), 6.82 (bs, IH), 4.93 (q, IH), 3.48 (d, 2H), 3.22-2.93 (m, 4H), 2.76 (m, 2H), 2.11 (s, 3H), 1.91-1.79 (m, 2H), 1.62-1.51 (m, IH), 1.49 (d, 3H), 1.38-1.24 (m, IH).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 50595-15-8, tert-Butyl 2-hydroxyacetate.

Reference:
Patent; VENENUM BIODESIGN LLC; HUANG, Chia-Yu; SHI, Dongchuan; KULTGEN, Steven G.; MCGUINNESS, Brian F; LETOURNEAU, Jeffrey J.; COLE, Andrew G.; BEASLEY, James R.; (358 pag.)WO2018/5801; (2018); A2;,
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Reference of 96-35-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 96-35-5, name is Methyl 2-hydroxyacetate, molecular formula is C3H6O3, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

Example 1Reduction of Methyl Glycolate in Methanol to Ethylene Glycol The following example shows the positive effect of adding a promoter to the catalyst mixture. Run 1 in the table below is a comparative example. Runs 2-9 represent variants of the current invention.A 300-milliliter autoclave was charged with Ru(Acac)3 (0.10 mmole), TRIPHOS (0.50 mmole), and the promoter in the amount specified in the table. Methanol (32 milliliters) and methyl glycolate (0.156 mole) were added, and the reactor was sealed under N2. The reactor was pressurized to 250 psig (1.7 MPa) with H2 and heated to 200 C. Upon reaching 200 C., the H2 pressure was raised to 2000 psig (13.8 MPa). The autoclave was stirred and held at 200 C., 2000 psig (13.8 MPa) for a total of 3 hours. The autoclave was then cooled, excess gas vented, and the contents recovered. The contents were analyzed by the use of an internal standard gas chromatography method for the presence of methyl glycolate (?MG?) and ethylene glycol (?EG?). The results are shown in the table below. Catalyst Activity Rate Amount of Conversion of Selectivity to (moles EG per Promoter MG EG mole of Ru Run Promoter (mmole) (%) (%) per hr) 1 none none 39.5 88.4 205 2 Zn 0.25 49.3 88.9 228 Acetonylacetonate 3Me4NBF4 0.025 99.7 98.2 509 4Me4NBF4 0.001 96.8 98.2 394 5NH4PF6 0.025 100 96.9 504 6NH4OAc 0.150 67.8 94.8 334 7Ph4PBr 0.025 84.1 97.8 428 8NaPh4B 0.500 81.1 93.5 394 9BuN4PF6 0.025 97.8 95.8 487 Analysis of the run without a promoter showed a 39.5% conversion of the methyl glycolate with 88.4% selectivity to ethylene glycol. The catalyst activity rate for this experiment was 205 moles of EG per mole of ruthenium per hour. On the other hand, runs with a promoter showed MG conversions of 49-100%, EG selectivities of 89-98%, and catalyst activity rates of 230-510 moles of EG per mole of ruthenium per hour. This data show the positive effects of adding a promoter to the reaction mixture.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 96-35-5, Methyl 2-hydroxyacetate.

Reference:
Patent; EASTMAN CHEMICAL COMPANY; US2009/143612; (2009); A1;,
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With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.2002-24-6, name is 2-Aminoethanol hydrochloride, molecular formula is C2H8ClNO, molecular weight is 97.544, as common compound, the synthetic route is as follows.name: 2-Aminoethanol hydrochloride

A dichloromethane (5 ml) solution of the [6-[(4-chlorophenylsulfonyl)(2,5-difluorophenyl)methyl]pyridin-3-yl]carboxylic acid (100 mg, 0.236 mmol) obtained in Example 50 were added triethylamine (80 mul, 0.566 mmol), 4-dimethylaminopyridine (15 mg, 0.118 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (54 mg, 0.283 mmol) and ethanolamine hydrochloride (28 mg, 0.283 mmol). The resulting mixture was stirred at room temperature for 17.5 hours. The reaction mixture was diluted with dichloromethane. The diluted mixture was washed sequentially with water, a saturated aqueous solution of sodium bicarbonate and brine. The organic layer thus obtained was dried over magnesium sulfate and concentrated under reduced pressure. The residue thus obtained was subjected to flash silica gel column chromatography. The fraction obtained from the dichloromethane_methanol=30:1 eluate was concentrated under reduced pressure to give the title compound (69 mg, 0.148 mmol, 63%) as a white powder. 1H-NMR (400MHz, CDCl3) delta: 2.38 (1H,t, J=4.9Hz), 3.65 (2H,td, J=5.4, 4.9Hz), 3.85 (2H,q, J=4.6Hz), 5.99 (1H,s), 6.77 (1H,brs), 6.90-6.96 (1H,m), 7.00-7.06 (1H,m), 7.42 (2H,d, J=8.6Hz), 7.56 (2H,d, J=8.6Hz), 7.70 (1H,d, J=8.1Hz), 7.97-8.01 (1H,m), 8.15 (1H,dd, J=8.1, 2.2Hz), 8.99 (1H,d, J=2.2Hz)H,m), mp: 179 to 181C. Elemental Analysis for C21H17ClF2N2O4S: Calculated: C,54.02; H, 3.67; Cl, 7.59; F,8.14; N,6.00; S,6.87. Found: C, 53.83; H,3.63; Cl, 7.72; F, 8.14; N,6.06; S, 7.02.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,2002-24-6, 2-Aminoethanol hydrochloride, and friends who are interested can also refer to it.

Reference:
Patent; DAIICHI PHARMACEUTICAL CO., LTD.; EP1640366; (2006); A1;,
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Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 71176-54-0, name is (5-Amino-1,3-phenylene)dimethanol. This compound has unique chemical properties. The synthetic route is as follows. Computed Properties of C8H11NO2

Compound 23 (5.6 g, 18.52 mmol) was dissolved in DCM (118 mL) andmethanol (58.8 mL). Diol24 (2.70 g, 17.64 mmol) and EEDQ (8.72 g, 35.3 mmol) wereadded and the reaction was stirred at rt overnight. The reaction mixture was concentratedand ethyl acetate was added to the residue. The resulting slurry was filtered, washed with ethyl acetate and dried under vacuum/N2 to give compound 25 as a white solid(2.79 g, 36percent yield). 1H NMR (400 MHz, DMSO-d6): 8 9.82 (s, 1H), 8.05, (d, 1H, J =9.2 Hz), 8.01 (d, 1H, J = 7.2 Hz), 7.46 (s, 2H), 6.95 (3, 1H), 5.21-5.12 (m, 2H), 4.47-4.42 (m, 4H), 4.40-4.33 (m, 1H), 4.33-4.24 (m, 1H), 3.58 (s, 3H), 2.33-2.26 (m, 2H),2.16-2.09 (m, 2H), 1.54-1.46 (m, 4H), 1.30 (d, 3H, J = 7.2 Hz), 1.22 (d, 3H, J = 4.4 Hz). LCMS = 2.894 min (8 min method). Mass observed (ESI+): 438.20 (M+H).

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, 71176-54-0, (5-Amino-1,3-phenylene)dimethanol.

Reference:
Patent; IMMUNOGEN, INC.; MILLER, Michael, Louis; SHIZUKA, Manami; (163 pag.)WO2018/195243; (2018); A1;,
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Related Products of 2568-33-4, Adding some certain compound to certain chemical reactions, such as: 2568-33-4, name is 3-Methylbutane-1,3-diol,molecular formula is C5H12O2, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 2568-33-4.

Toluene-4-sulfonic acid 3-hydroxy-3-methyl-butyl ester 3-Methyl-1,3-butanediol (1.5 mL, 14.1 mmol) is suspended in dry dichloromethane (5 mL) and pyridine (1.24 mL, 15.46 mmol) is added followed by 4-toluenesulfonyl chloride (2.68 g, 14.1 mmol). The mixture is stirred overnight then washed with 1 M aqueous hydrochloric acid, dried and the solvent removed under vacuum. The residue is purified by flash chromatography (0-30% ethyl acetate in cyclohexane) to give the title compound. (Yield 970 mg). LC (METHOD 2): tR=5.67 min; Mass spectrum (ES+): m/z=258 [M+H]+.

According to the analysis of related databases, 2568-33-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; LINGARD, Iain; HAMPRECHT, Dieter; US2015/148347; (2015); A1;,
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Application of 33524-31-1 ,Some common heterocyclic compound, 33524-31-1, molecular formula is C9H12O3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.

General procedure: A mixture of the benzylic alcohol 1 (1 mmol) and 98% H2SO4 (1 mmol) in DMSO (3 mL) was stirred for the appropriate time under reflux conditions. The mixture was then cooled to r.t., and brine (4 mL) was added. The organic phase was extracted with CH2Cl2 (6 mL), and the organic layer was dried (Na2SO4), filtered, and concentrated under reduced pressure. In all cases, the reaction products were obtained with high purity, and did not require further purification by distillation or column chromatography.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,33524-31-1, its application will become more common.

Reference:
Article; Sheikhi, Ehsan; Adib, Mehdi; Karajabad, Morteza Akherati; Gohari, Seyed Jamal Addin; Synlett; vol. 29; 7; (2018); p. 974 – 978;,
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