Alcohols-buliding-blocks

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. 647-42-7, name is 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol. A new synthetic method of this compound is introduced below., 647-42-7

The corresponding fluoroalcoholic substrate 1e (0.728 g, 2.0 mmol) was added to the reaction flask and anhydrous DMF (3 mL) was added.Additional DSC (0.613 g, 1.2 eq.) and pyridine (0.16 mL, 1.0 eq.).The mixture was heated at 40 C for 15 h.It was monitored by TLC until the alcohol was completely reacted. Cool the mixture to room temperature,Boc-t-Bu-lysine (0.604 g, 2.0 mmol) was added.Keep the temperature below 30 C.The reaction mixture was then stirred at room temperature overnight.It was monitored by TLC until the starting material was complete.Water (10 mL) and ethyl acetate (10 mL) were added to the mixture.The organic layer was separated and the aqueous layer was evaporated elutCombine the two organic layers, using 1 mol/L hydrochloric acid in sequence.Wash with water and saturated brine,It was dried over anhydrous magnesium sulfate. Concentrate the organic solution,Fluorine-containing amino acid derivative precursor obtained by flash column chromatography3e (0.598g, 1.86mmol),The yield is 93%.Purity is 99%,It is an oily substance.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,647-42-7, 3,3,4,4,5,5,6,6,7,7,8,8,8-Tridecafluorooctan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; Shanghai Institute of Technology; Liu Meina; Zhu Yu; Wu Tong; Deng Wei; Xuan Maojie; Miao Dengyun; Liu Zhifeng; Shan Yu; (13 pag.)CN108997168; (2018); 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. 56239-26-0, name is cis-4-Aminocyclohexanol hydrochloride. This compound has unique chemical properties. The synthetic route is as follows. 56239-26-0

EXAMPLE 86[0124] Preparation of 4-((R)-Tetrahydrofuran-3-yloxy)-5-(2,3- dihydrobenzo[b][l,4]dioxin-6-yl)-N-((ls,4S)-4-methoxycyclohexyl)pyrimidin-2-amineJ.: Preparation of Starting Material 4-Methoxycyclohexanamine HydrochlorideReagents and Conditions: a) K2CO3 H2; b) KHMDS, MeI, and THF; c) NH2NH2, EtOH, then 4M HCI H2N HCIStep 1-1: Preparation of 2-((ls,4s)-4-Hydroxycyclohexyl)isoindoline-l,3-dione (2) [0125] To a stirred solution of cis-4-aminocyclohexanol HCl (107 mg, 0.71 mmol) in H2O(1.7 mL) at room temperature was added K2CO3 (174 mg, 1.25 mmol), followed by N- carboethoxyphthalimide (174 mg, 0.79 mmol). After stirring at room temperature for 30 min, the solid was filtered, washed with H2O, and dried in vacuo to provide the title compound (140 mg, 81percent) as a white solid. 1H NMR (300 MHz, CDCl3) delta 7.82 (m, IH), 7.79 (m, IH), 4.10 (m, IH), 2.64 (m, IH), 1.5-2.0 (set of m, 4H). MS (ESI) m/z: Found: 491 (2M+ + 1), CaIc. 245(M+).

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, 56239-26-0, cis-4-Aminocyclohexanol hydrochloride.

Reference:
Patent; CYSTIC FIBROSIS FOUNDATION THERAPEUTICS, INC.; CHIANG, Phoebe; GHOSH, Shomir; WO2010/68863; (2010); A2;,
Alcohol – Wikipedia,
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112-70-9, 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. 112-70-9, name is 1-Tridecanol. This compound has unique chemical properties. The synthetic route is as follows.

Example 3 In the same manner as Example 1 except using 600 parts of tridecyl alcohol, 2.2 parts of water, 240 parts of allyl chloride and 335 parts of triethyl amine, in place of 570 parts of lauryl alcohol, 5 parts of sodium hydroxide, 275 parts of allyl chloride and 375 parts of triethyl amine, was obtained 960 parts of lauryl allyl maleate of 97.1% purity and of Gardner Color 3. A molar ratio of maleic anhydride:lauryl alcohol was 1:1, and maleic acid monolauryl ester:allyl chloride:triethyl amine:water was 1:1.05:1.10:0.04.

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, 112-70-9, 1-Tridecanol.

Reference:
Patent; Sanyo Chemical Industries, Ltd.; US5523465; (1996); A;,
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124-68-5, 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. 124-68-5, name is 2-Amino-2-methyl-1-propanol, molecular formula is C4H11NO, 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.

2-amino-2-methyl-1-propanol (4.5g,50.56mmol), sodium bicarbonate (8.4g, 100mmol) and sodium carbonate (10.6g, 100mmol) were mixed in a 250mLreaction flask,, a mixture of dioxane and water (160mL, 3:1) was added, the reaction solution was cooled below 0Cunder an ice bath, a solution of di-tert-butyl dicarbonate (13.1g, 59.82mmol) in dioxane (5mL) was added dropwise under stirring. After completion of the addition, the reaction solution was stirred for 6 hours. After completion of the reaction,dioxane was evaporated under reduced pressure, the residue was extracted with ethyl acetate. The organic phase waswashed with saturated brine, dried over anhydrous sodium sulfate and concentrated. The residue was purified by silicagel column chromatography to give 8.2g product with a yield of 85.77%.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 124-68-5, 2-Amino-2-methyl-1-propanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Shanghai Pharmaceuticals Holding Co., Ltd.; XIA, Guangxin; LI, Di; ZUO, Hongjian; WU, Guangsheng; DUAN, Lingjun; ZHANG, Jing; MAO, Yu; LIU, Yanjun; (152 pag.)EP3424928; (2019); A1;,
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4654-39-1 ,Some common heterocyclic compound, 4654-39-1, molecular formula is C8H9BrO, 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.

A solution of 2-(4-bromophenyl)ethanol (342 mul, 2.50 mmol), DIEA (653 mul, 3.75 mmol) and methanesulfonyl chloride (213 mul, 2.70 mmol) in DCM (12 ml) was stirred 1 h 30 at 0 C. and then overnight at rt. The solution was diluted with DCM, washed with a 0.5 N solution of HCl and brine. The organic phase was dried over Na2SO4 and concentrated to afford a yellow oil (700 mg, 100%).

According to the analysis of related databases, 4654-39-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; The Scripps Research Institute; Kamenecka, Theodore Mark; Griffin, Patrick R.; Shin, Youseung; He, Yuanjun; Blayo, Anne-Laure; Lyda, Brent R.; Koenig, Marcel; Kumar, Naresh; Burris, Thomas; (119 pag.)US9586928; (2017); B2;,
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100-37-8, 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. 100-37-8, name is 2-(Diethylamino)ethanol. This compound has unique chemical properties. The synthetic route is as follows.

j0044] Example 2: a bis (2-diethylaminoethyl) ether synthesizing method using N,N-diethylethanolamine, diethylamine and ethyne as raw materials (original raw materials) is performed by the following steps in proper order:10045] step 1: synthesizing:10046] wherein at a room temperature, 117 g N,N-diethylethanolamine (1.0 mol), 268 g diisobutyl ether (as a solvent) and 3.6 g sodium ethoxide are added in a high-pressure reaction dave with a mixing and temperature-measuring device; the dave cover is put on and leakage is inspected; then 6.5 g ethyne (0.25 mol) and 55.0 g diethylamine (0.75 mol) are forced into the dave in proper order; afier feeding, a temperature is raised to 50 C., and kept on for 7 h before completing the reaction;10047] afier reaction, the dave is opened and a filtrate is obtained by filtering the reaction mixture; and step 2:10048] distilling the filtrate obtained at 60 C. and atmospheric pressure for half an hour for the unreacted diethylamine to come out; then proceeding to rectification at reduced pressure intermittently; at a pressure of 1 kPa, collecting the previous fractions (all fractions before 91 C.)- unreacted N,N-diethylethanolamine and solvent; then collecting the fractions at 9 1-93 C. and obtaining bis (2-diethylaminoethyl) etherweighing 51.5 g; wherein a product purity is 99.1%; by taking the consumed ethyne as reference, a yield rate is 95.3%.

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 100-37-8, 2-(Diethylamino)ethanol.

Reference:
Patent; SICHUAN ZHIJIANG ADVANCED MATERIALS CO., LTD.; Zhang, Chao; Zhang, Hua; Ye, Xiaoming; Zhang, Qi; Ye, Chuanwei; US2015/291506; (2015); A1;,
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702-98-7, 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. 702-98-7, name is 2-Methyladamantan-2-ol. This compound has unique chemical properties. The synthetic route is as follows.

An autoclave was charged with 2,3-dibromo-1,1,1-trifluoropropane (0.2559 g, 1.0 mmol), 2-methyl-2-adamantanol (0.249 g, 1.5 mmol), triethylamine (0.202 g, 2.0 mmol), lithium carbonate(0.0369 g, 0.5 mmol), dichlorobis (triphenylphosphine) palladium(II) (0.0070 g, 0.01 mmol), and tetrahydrofuran (2.0 mL), which were then stirred at 100C for 15 hours after introducing carbon monoxide (1.0 MPaG). After the end of the reaction, the autoclave was cooled, ventilated, and added with benzotrifluoride as an internal standard substance, followed by stirring and leaving still for a while to let a salt precipitate. Quantification using a 19F-NMR integration value revealed that 2-trifluoromethyl acrylic acid 2-methyl-2-adamantyl ester was obtained with a yield of 91.1% on the basis of 2,3-dibromo-1,1,1-trifluoropropane.

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 702-98-7, 2-Methyladamantan-2-ol.

Reference:
Patent; Tosoh F-Tech, Inc.; SAGAMI CHEMICAL RESEARCH CENTER; EP1637514; (2006); A1;,
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106-28-5, 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 106-28-5 as follows.

Step 4: A 3-N 100 mL flask was charged with PCl3 (2.8 mL, 31.6 mmol) and dry DMF (32 mL) then stirred at RT for 1 h. In a separate 50 mL flask, farnesol (Ex-1B-5) (10.0 g, 45.2 mmol) and DMF (10 mL) was charged. The PCl3/DMF solution was then transferred to the farnesol, solution and the resulting dark orange solution was stirred for 1 h. The reaction was quenched by addition of solid NaHCO3 (2.5 g, 63.2 mmol). The solvent was removed by high vacuum rotary evaporation to yield an oily orange residue. To the residue was added MTBE (40 mL) and water (40 mL). The aqueous phase was washed with MTBE (3¡Á20 mL). The MTBE layers were combined, washed with brine (2¡Á20 mL), dried over MgSO4, filtered and finally concentrated by rotary evaporation to yield 1-chloro-3,7,11-trimethyl-dodeca-2,6,10-triene (Ex-1B-6) as a yellow oil (9.89 g, 92%). 1H NMR (400 MHz, CDCl3) delta (ppm): 5.47 (broad-t, J=8.3 Hz, 1 H), 5.15-5.07 (m, 2 H), 4.12 (d, J=8.1 Hz, 2 H), 2.18-1.95 (m, 8 H), 1.75 (s, 3 H), 1.70 (s, 3 H), 1.62 (s, 6 H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,106-28-5, its application will become more common.

Reference:
Patent; Miller, Guy M.; Hecht, Sidney M.; US2006/281809; (2006); A1;,
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A common compound: 6338-55-2, name is 2-(2-(2-Aminoethoxy)ethoxy)ethanol,molecular formula is C6H15NO3, it can change the direction of chemical reaction, and react with certain compounds to generate new functional products. A new synthetic method of this compound is introduced below., 6338-55-2

General procedure: The desired aminoalcohol (17 mmol, 2-(2-aminoethoxy)ethanol or 2-[2-(2-aminoethoxy)ethoxy]ethanol) was dissolved in CH3OH (10 mL) and TEA (5.45 mL, 39.2 mmol) was added. To this solution, stirred at room temperature, was added dropwise a solution of benzyloxycarbonyl chloride (ZCl, 3.2 g, 18.77 mmol) in CH3OH (5 mL). After the addition was complete the reaction mixture was stirred at room temperature for 20 h, protected from moisture with a CaCl2 drying tube. The solvent was then evaporated and the crude was dissolved in CH2Cl2 (150 mL) and washed first with a 5% aqueous solution of KHSO4 (2 ¡Á 50 mL) and then with water (2 ¡Á 50 mL). The evaporation of the dried solvent (Na2SO4) afforded the product as a clear oil pure enough to be used in the following steps.

With the rapid development of chemical substances, we look forward to future research findings about 6338-55-2.

Reference:
Article; Sissi, Claudia; Dovigo, Luca; Greco, Maria Laura; Ciancetta, Antonella; Moro, Stefano; Trzci?ski, Jakub W.; Mancin, Fabrizio; Rossi, Paola; Spalluto, Giampiero; Tecilla, Paolo; Tetrahedron; vol. 73; 21; (2017); p. 3014 – 3024;,
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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 346-06-5 as follows., 346-06-5

Step A: Preparation of 2-(2-(trifluoromethyl)phenyl)furo[2,3-c]pyridin-3-amine: To an ice cooled (0¡ã C.) suspension of NaH (61.93 mg, 1.548 mmol) in DMF (5 mL) was added (2-(trifluoromethyl)phenyl)methanol (0.2262 mL 1.703 mmol) and the reaction mixture was stirred 10 minutes. 3-Bromoisonicotinonitrile (283.4 mg, 1.548 mmol) in 5 mL DMF was added, and the reaction mixture was stirred overnight while warming to 60¡ã C., then cooled to room temperature, diluted with water and EtOAc, and the layers were separated. Purification by column chromatography (10percent MeOH/CH2Cl2) provided 67 mg (15percent) of the desired product. MS (APCI-pos) M+1=279.5.

The chemical industry reduces the impact on the environment during synthesis 346-06-5, I believe this compound will play a more active role in future production and life.

Reference:
Patent; Miknis, Greg; Lyssikatos, Joseph P.; Laird, Ellen; Tarlton, Eugene; Buckmelter, Alexandre J.; Ren, Li; Rast, Bryson; Schlacter, Stephen T.; Wenglowsky, Steven Mark; US2007/49603; (2007); A1;,
Alcohol – Wikipedia,
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