Tag: M.W=100-200

Reference of 5259-98-3, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 5259-98-3, name is 5-Chloropentan-1-ol. A new synthetic method of this compound is introduced below.

To a solution of benzylamine (0.66?mL, 6.03?mmol) and 5-chloropentan-1-ol (0.42?mL, 4.02?mmol) in 5?mL of anhydrous acetonitrile, 555?mg of K2CO3 (4.02?mmol) were added. The mixture was stirred at 80?°C for 48?h and concentrated in vacuo. The residue was dissolved with CH2Cl2, and the organic layer was washed twice with a solution of 10percent NaOH, dried on Na2SO4 and evaporated to give the crude product that was purified by flash chromatography, using CH2Cl2/MeOH/NH4OH 95:5:0.5 as eluting system. 160?mg (20.6percent) of title compound as a yellow oil were obtained. 1H NMR (CDCl3) delta: 7.33-7.26 (m, 5H, CH arom.); 3.78 (s, 2H, NCH2Ph); 3.61 (t, J?=?6.4?Hz, 2H, CH2OH); 2.65 (t, J?=?6.8?Hz, 2H, NCH2); 1.88 (s, 1H, NH); 1.61-1.50 (m, 4H, CH2); 1.47-1.42 (m, 2H, CH2) ppm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,5259-98-3, its application will become more common.

Reference:
Article; Dei, Silvia; Romanelli, Maria Novella; Manetti, Dina; Chiaramonte, Niccolo; Coronnello, Marcella; Salerno, Milena; Teodori, Elisabetta; Bioorganic and Medicinal Chemistry; vol. 26; 1; (2018); p. 50 – 64;,
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Related Products of 84832-00-8 ,Some common heterocyclic compound, 84832-00-8, molecular formula is C7H8FNO, 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.

Intermediate 4; (2-Flu or o-5-hvdrazinylphenyl)methanol hydrochloride; (5-Amino-2-fluorophenyl)methanol (3.6 g, 25.8 mmol) was dissolved in cone. HCl (39 ml) and cooled to 00C. A solution OfNaNO2 (1.89g, 27.4 mmol) in water (9.4 ml) was added dropwise during 20 minutes at O0C. The mixture was stirred for 15 minutes and a solution of SnCl2 (1 Ig, 57.4 mmol) in cone. HCl (11.5 ml) was added dropwise. The mixture was allowed to stir for 60 minutes at O0C and basified by addition of aqueous 14N NaOH and extracted with EtOAc. The organic phase was washed with brine and extracted with a solution of HCl (1 M). The water phase was freeze-dried to give the title compound (1.65 g, 33%). APCI-MS m/z: 157 [MH+].

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,84832-00-8, its application will become more common.

Reference:
Patent; ASTRAZENECA AB; WO2009/82342; (2009); A1;,
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Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 28539-02-8, name is 1-(Hydroxymethyl)benzotriazole. A new synthetic method of this compound is introduced below., Quality Control of 1-(Hydroxymethyl)benzotriazole

To a stirred solution of n-BuLi (2.5 M in hexanes, 22.9 ml, 57.4 mmol) in THF(120 ml) was added dropwise iPr2NH (8.11 ml, 57.4 mmol) at -10 C. The solution was allowed to stir at 0 C for 30 min and then cooled to -78 C. Enone 83 (8.62 g, 19.1 mmol) inTHF (25 ml) was added and stirring was continued for 1 h. 1H-Benzotriazole-1-methanol in THF (175 ml) was added dropwise and the reaction mixture was kept 2 h at -78 C. The reaction was quenched with water (85 ml) and extracted with Et2O (2 × 250 ml). The combined organic layers were washed successively with 4 M NaOH (85 ml) and brine (85 ml), dried (MgSO4) and concentrated in vacuo. Purification by flash chromatography onsilica gel with petroleum ether/EtOAc 9:1 to 6:1 as eluent gave alcohol S28 (6.10 g, 67%) as a colourless oil.

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, 28539-02-8, 1-(Hydroxymethyl)benzotriazole.

Reference:
Article; Bruss, Hanna; Schuster, Hannah; Martinez, Remi; Kaiser, Markus; Antonchick, Andrey P.; Waldmann, Herbert; Beilstein Journal of Organic Chemistry; vol. 10; (2014); p. 194 – 208;,
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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.495-76-1, name is Benzo[d][1,3]dioxol-5-ylmethanol, molecular formula is C8H8O3, molecular weight is 152.1473, as common compound, the synthetic route is as follows.category: alcohols-buliding-blocks

General procedure: To a solution of Cu(OAc)2 (0.025 mmol, 0.0046 g) and potassium tert-butoxide (0.175 g, 2.5 mmol) in anhydrous dioxane (3 mL), the corresponding amine 1 (2.5 mmol) or the triphenylphosphoranylidenaniline 18 (2.5 mmol) and the correspondent alcohol 2 or 4 (3.75 mmol) were added successively under inert argon atmosphere. After 2 or 5 days of reaction at 130 C (see Table 2 and Scheme 2), the resulting mixture was hydrolyzed with a saturated solution of ammonium chloride (10 mL). The mixture was extracted with AcOEt (3×10 mL) and washed with brine (10 mL), after drying with anhydrous MgSO4, was filtered on Celite and the solvents were removed under low pressure(15-18 Torr). The resulting mixture was purified by column chromatography (if needed).

At the same time, in my other blogs, there are other synthetic methods of this type of compound,495-76-1, Benzo[d][1,3]dioxol-5-ylmethanol, and friends who are interested can also refer to it.

Reference:
Article; Martinez-Asencio, Ana; Ramon, Diego J.; Yus, Miguel; Tetrahedron; vol. 67; 17; (2011); p. 3140 – 3149;,
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Adding a certain compound to certain chemical reactions, such as: 349-95-1, (4-(Trifluoromethyl)phenyl)methanol, 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, HPLC of Formula: C8H7F3O, blongs to alcohols-buliding-blocks compound. HPLC of Formula: C8H7F3O

General procedure: Under an N2 atmosphere, a mixture of secondary alcohol (0.5 mmol), primary alcohol (0.6 mmol), 1a (5 mol %), NaOH (0.1 mmol), 4 A molecular sieve (0.6 g), and toluene (1.5 mL) was added into a 25 mL Schlenk tube equipped with a stirring bar. The mixture was heated to 120 C under a slow and steady N2 flow for 24 h. After cooling to ambient temperature, 6 mL water was added and the aqueous solution extracted with ethyl acetate (3 x 5 mL). The combined extracts were dried over anhydrous Na2SO4, and concentrated under reduced pressure. The crude product purified on a short flash chromatography column.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,349-95-1, (4-(Trifluoromethyl)phenyl)methanol, and friends who are interested can also refer to it.

Reference:
Article; Zhang, Shi-Qi; Guo, Bin; Xu, Ze; Li, Hong-Xi; Li, Hai-Yan; Lang, Jian-Ping; Tetrahedron; vol. 75; 47; (2019);,
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Synthetic Route of 27489-62-9, 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. 27489-62-9, name is trans-4-Aminocyclohexanol, molecular formula is C6H13NO, 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.

5-Fluoro-2-nitrobenzotrifluoride (400 mg, 1.91 mmol) and trans-4- aminocyclohexanol (220 mg, 1.91 mmol) are dissolved in dimethylsulfoxide (10 mL) and the reaction is then heated at 95C for 3.5 hours. After cooling to room temperature, the mixture is diluted with dichloromethane (15 mL) and washed with water (3 x 10 mL). The organic phase is collected and dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude product is recrystallised from petrol ether. The desired product is finally isolated as a yellow solid (84% yield).

According to the analysis of related databases, 27489-62-9, the application of this compound in the production field has become more and more popular.

Reference:
Patent; INTERVET INTERNATIONAL B.V.; CHASSAING, Christophe Pierre Alain; MEYER, Thorsten; WO2010/146083; (2010); A1;,
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Related Products of 455-01-6, 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 455-01-6 as follows.

Example 82 3-(Trifluoromethyl)phenethyl N-{4-[(6,7-dimethoxy-4-quinolyl)oxy]phenyl}carbamate 4-[(6,7-Dimethoxy-4-quinolyl)oxy]aniline (72 mg) was added to toluene/triethylamine = 10/1 (7 ml), and the mixture was heated under reflux to prepare a solution. A solution of triphosgene (125 mg) in methylene chloride was then added to the solution, and the mixture was heated under reflux for 15 min. Subsequently, 3-trifluoromethylphenethyl alcohol (70 mg) was added thereto, and the mixture was further stirred with heating under reflux for 2 hr. After the completion of the reaction, the reaction solution was allowed to cool to room temperature before distilled water was added thereto. The mixture was subjected to separatory extraction with chloroform, followed by washing with a 1 N aqueous hydrochloric acid solution and saturated brine. The washed solution was dried over sodium sulfate and was concentrated. The residue was purified on a column using chloroform/methanol to give the title compound (101 mg, yield 76%). 1H-NMR (CDCl3, 400 MHz): 8.42 – 8.49 (1H, m), 8.12 (1H, s), 7.61 (1H, s), 7.42 – 7.59 (6H, m), 7.13 – 7.18 (2H, m), 6.76 (1H, s), 6.66 (1H, d, J = 6.6 Hz), 4.44 (2H, t, J = 6.7 Hz), 4.15 (3H, s), 4.08 (3H, s), 3.07 (2H, t, J = 6.7 Hz) Mass spectrometry value (ESI-MS, m/z): 513 (M++1)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,455-01-6, its application will become more common.

Reference:
Patent; KIRIN BEER KABUSHIKI KAISHA; EP1243582; (2002); 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.431-38-9, name is 3-Amino-1,1,1-trifluoropropan-2-ol, molecular formula is C3H6F3NO, molecular weight is 129.0811, as common compound, the synthetic route is as follows.Recommanded Product: 3-Amino-1,1,1-trifluoropropan-2-ol

General procedure: Sodium triacetoxyhydroborate (900 mg, 4.2 mmol) was added to a solution of 1-naphthaldehyde (2.8 mmol) and the amine (2.8 mmol) in 1,2-dichloroethane (80 mL) at r.t. under nitrogen atmosphere. The reaction mixture was stirred for 6 h at r.t. and was quenched with sat. aq. NaHCO3 (20 mL) and extracted with DCM (3 x 50 mL). The combined organic layer was washed with brine (50 mL), dried and evaporated. The compound was purified by preparative HPLC on a XBridge C18 column (10 m 250×19 ID mm) using a gradient of 30-80% Acetonitrile in H2O/ACN/NH3 95/5/0.2 buffer over 20 minutes with a flow of 19 mL/min. The compounds were detected by UV at 220 nm to provide the product.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,431-38-9, 3-Amino-1,1,1-trifluoropropan-2-ol, and friends who are interested can also refer to it.

Reference:
Article; Giordanetto, Fabrizio; Wallberg, Andreas; Ghosal, Saswati; Iliefski, Tommy; Cassel, Johan; Yuan, Zhong-Qing; Von Wachenfeldt, Henrik; Andersen, Soren M.; Inghardt, Tord; Tunek, Anders; Nylander, Sven; Bioorganic and medicinal chemistry letters; vol. 22; 21; (2012); p. 6671 – 6676,6;,
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Electric Literature of 770-71-8 , The common heterocyclic compound, 770-71-8, name is Adamantan-1-ylmethanol, molecular formula is C11H18O, 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.

The adamantane 4-methylbenzenesulfonate was synthesized by reacting adamantyl alcohol (20.5 g, 123 mmol) with p-toluenesulfonic chloride (23.6 g, 123 mmol) in 75 mL of regular DCM, in the presence of 25 mL of triethylamine for 48 hours at room temperature. More DCM was added (100 mL) and the organic layer was washed with water (3×100 mL). Drying, (MgSO4), and evaporation of the solvent gave 34.5 g of tea color oil which under trituration with hexane afforded white solid adamantane 4-methylbenzenesulfonate (30.5 g, 76%).

The synthetic route of 770-71-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NITTO DENKO CORPORATION; RACHWAL, MILA; YAMAMOTO, MICHIHARU; (134 pag.)JP2016/509621; (2016); A;,
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Application of 671802-00-9 ,Some common heterocyclic compound, 671802-00-9, molecular formula is C9H18O4, 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.

Compound 16-3 (2.0 g, 10.5 mmol), N-hydroxyphthalimide (2.05 g, 12.6 mmol) and triphenylphosphine (3.58 g, 13.65 mmol) were dissolved in 50 mL of tetrahydrofuran followed by addition of DIAD (3.26 mL, 15.75 mmol) at 0C. The resulting solution was stirred at room temperature overnight, and then concentrated to dryness. The residue was purified by flash column chromatography to give compound 16-5.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,671802-00-9, its application will become more common.

Reference:
Patent; AMBRX, INC.; MIAO, Zhenwei; ATKINSON, Kyle, C.; BIROC, Sandra; BUSS, Timothy; COOK, Melissa; KRAYNOV, Vadim; MARSDEN, Robin; PINKSTAFF, Jason; SKIDMORE, Lillian; SUN, Ying; SZYDLIK, Angieszka; VALENTA, Ianina; WO2012/166560; (2012); A1;,
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