Month: January 2021

Synthetic Route of 2043-47-2 ,Some common heterocyclic compound, 2043-47-2, molecular formula is C6H5F9O, 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.

Mixing 5.00 parts of the salt represented by the formula (I-1-c) and 25 parts of chloroform;Stirred at 23 C. for 30 minutes.In the mixture obtained,1.09 parts of a compound represented by the formula (I-1-d) is added,Furthermore, it stirred at 50 degreeC for 2 hours.After cooling the resulting reaction mixture to 23 C.2.67 parts of a compound represented by formula (I-1-e) are added,Furthermore, it stirred at 23 degreeC for 18 hours. After adding 50 parts of chloroform and 50 parts of ion-exchanged water to the obtained reaction mixture and stirring for 30 minutes at 23 C., the layers were separated to take out the organic layer.In the organic layer obtained,After adding 25 parts of a 5% aqueous solution of oxalic acid and stirring at 23 C. for 30 minutes,The layers were separated and the organic layer was taken out.After adding 25 parts of ion-exchanged water to the obtained organic layer and stirring at 23 C. for 30 minutes,Separated and took out the organic layer. This water washing operation was repeated 5 times.After filtering the obtained organic layer,The filtrate is concentrated to a concentrated residue,By adding 30 parts of tert-butyl methyl ether and stirring at 23 C. for 30 minutes, the supernatant is removed and concentrated by4.39 parts of a salt represented by the formula (I-1) were obtained.

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. 2043-47-2, 1H,1H,2H,2H-Nonafluoro-1-hexanol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Sumitomo Chemical Co., Ltd.; Komuro, Katsuhiro; Takahashi, Yuki; Ichikawa, Koji; (96 pag.)JP2019/59712; (2019); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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. 115-20-8, name is Trichloroethanol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 115-20-8

Compound 1 (2g, 13.4mmol) was dissolved intetrahydrofuran (15ml) was added triethylamine (176mg), Was added dropwise to asolution of compound 2 (2.1g, 24.8mmol), dropwise addition was heated to 60 C under reflux, stirringStirred overnight. The reaction was stopped, after the reaction mixture wascooled added saturated citric acid (20ml), extracted with methylene chloride,The organic layer was washed with water, brine, dried over anhydrous NaSO 4,isolated by column chromatography to give compound 3 (2.2g, 71% yield).

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, 115-20-8, Trichloroethanol.

Reference:
Patent; ARROMAX PHARMATECH SUZHOU CO LTD; JIAN, HONG; XU, XIN; (12 pag.)CN104230792; (2016); B;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 2807-30-9, 2-Propoxyethanol, 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, 2807-30-9, blongs to alcohols-buliding-blocks compound. Formula: C5H12O2

Dimethyl 4-nitro-1H-pyrazole-3, 5-dicarboxylate (WO00/24745, page 48, preparation 2) (15g, 60mmol), 2-propoxyethanol (8.2mL,70mmol) and triphenylphosphine(18. 9g,70mmol) were dissolved in tetrahydrofuran(150mL) and the solution cooled to0 C. The solution was treated withdiisopropyl azodicarboxylate (14.2mL,70mmol) and the reaction mixture stirred at0 C for 3 hours before being allowed to warm to room temperature. The reaction mixture was concentrated in vacuo and the residue purified by column chromatography on silica gel eluting with ethyl acetate: pentane 15: 85 and then againeluting withdichloromethane to yield the title product. ‘H NMR (CD30D, 400MHz) a : 0.82 (t, 3H), 1.47 (q, 2H), 3.34 (t, 2H), 3.78 (t, 2H), 3.91 (s, 6H), 4.76 (t, 2H). MS APCI+ m/z 316 [MH] +

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2807-30-9, its application will become more common.

Reference:
Patent; PFIZER LIMITED; PFIZER INC.; WO2005/49616; (2005); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Reference of 456-47-3, 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. 456-47-3, name is 3-Fluorobenzyl alcohol, molecular formula is C7H7FO, 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-ChIoro- l-(3-fluorobenzyIoxy)-4-nitrob enzene (14) was prepared from (3-fluoro-phenyl)-methanol (13)(Aldrich) and 2-chloro-l-fluoro-4-nitro- benzene (12) (Aldrich) according to Wallace et al. (Preparation of cyanoguanidines and cyanoamidines as ErbB2 and EGFR inhibitors. 2005). Yield (20.Og; 85%) yellow crystals. 1H- NMR (DMSO-[D6]): delta (ppm) = 5.41 (s, 2H), 7.18-7.25 (m, H), 7.31-7.35 (m, 2H), 7.43-7.50 (m, 2H), 8.26 (dd, IH, J = 9.2 Hz, 4J – 2.8 Hz), 8.35 (d, IH, 4J = 2.8 Hz).

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 456-47-3, 3-Fluorobenzyl alcohol.

Reference:
Patent; 4SC AG; WO2009/63054; (2009); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a compound 5456-63-3, name is trans-2-Aminocyclohexanol hydrochloride. This compound has unique chemical properties. The synthetic route is as follows. category: alcohols-buliding-blocks

(0746) A solution of 6-(2′-hexyldecanoyloxy)hexan-l-al (2.4 g) and trans-2- aminocyclohexanol hydrochloride (0.35 g) in methylene chloride (10 (0747) mL)/tetrahydrofuran (10 mL) was treated with sodium triacetoxyborohydride (1.3 g) for 1.5 hours. The solution was washed with aqueous sodium hydrogen carbonate solution. The organic phase was dried over anhydrous magnesium sulfate, filtered and the solvent removed. The residue was passed down a silica gel column using a (0748) methanol/methylene chloride (0-8/100-92%)) gradient, yielding compound III-9 as colorless oil (0.6 g

With the rapid development of chemical substances, we look forward to future research findings about 5456-63-3.

Reference:
Patent; ACUITAS THERAPEUTICS, INC.; LIN, Paulo, Jia Ching; TAM, Ying; (211 pag.)WO2018/191719; (2018); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

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.101597-25-5, name is 1,1-Bis(4-methoxyphenyl)prop-2-yn-1-ol, molecular formula is C17H16O3, molecular weight is 268.31, as common compound, the synthetic route is as follows.HPLC of Formula: C17H16O3

The more polar product of Example 1, Step 4 (2,10-bistrifluoromethyl-7,7-dimethyl-5-hydroxy-7H-benzo[C]fluorene,2.6 grams), 1,1-bis-(4-methoxyphenyl)-2-propyn-1-ol (2.26 grams), 14 drops of methane sulfonic acid and 250mL of methylene chloride were combined in a reaction flask and stirred overnight under a nitrogen atmosphere. Thereaction mixture was washed carefully with a mixture of 250 mL of a saturated sodium bicarbonate solution and 250 mLof water. The organic layer was separated, dried over sodium sulfate, and concentrated by rotary evaporation to get abrown solid. This brown solid was purified via flash column chromatography on a silica gel column using a mixture ofhexane and ethyl acetate (80/20) as the eluant to yield 1.5 grams of an off white solid. A NMR spectrum showed theproduct to have a structure consistent with 3,3-bis-(4-methoxyphenyl)-7,10-bistrifluoromethyl-13,13-dimethyl-3H,13Hindeno[2.1-f]naphtho[1,2-b]pyran as represented by the following graphic formula

At the same time, in my other blogs, there are other synthetic methods of this type of compound,101597-25-5, 1,1-Bis(4-methoxyphenyl)prop-2-yn-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; TRANSITIONS OPTICAL INCORPORATED; CHOPRA, ENU; (24 pag.)KR101593284; (2016); B1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Adding a certain compound to certain chemical reactions, such as: 4461-39-6, N-(2-Hydroxyethyl)-1,3-propanediamine, 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, 4461-39-6, blongs to alcohols-buliding-blocks compound. Safety of N-(2-Hydroxyethyl)-1,3-propanediamine

In a nitrogen purged glove box, a 3-Liter, 4-neck round-bottom flask, fitted with a mechanical stirrer, thermocouple, nitrogen inlet adapter and septum, was charged with 2-(3- aminopropylamino)ethanol (144 g; 1.22 mol) and sulfolane (1.00 L; 10.5 mol). This was brought to a fume hood where it was attached to a nitrogen line and the septum was replaced with an adapter holding a 1/8 inch diameter Teflon tube attached to a HBr lecture bottle. While stirring, the hydrogen bromide (HBr) gas was admitted subsurface at a rate that allowed the temperature to rise to about 1300C. Addition was discontinued after heat evolution ceased and HBr was no longer absorbed; two equivalents had reacted, giving the dihydrobromide salt of the starting alcohol. The adapter on the reaction flask was replaced with a pressure-equalized dropping funnel containing phosphorus tribromide (PBr3) (132 g, 0.487 mol, 1.2 equiv) which was added over about 10 minutes at a temperature of between about 110 to about 130C. The solution was then stirred under nitrogen at 1200C for 20 minutes, after which time the product had crystallized into a thick cake. Additional sulfolaiie (380 mL) was added, resulting in a slurry which could be stirred at 120C. After a period of time, the hot slurry was transferred through a 3/8 ” polypropylene tube and was dropped into 2 L of acetone, stirring in a 4 L beaker (in three approximately equal portions) to precipitate the product. After each portion, the solid was filtered and rinsed with acetone and the beaker was charged with 2 L of fresh acetone for the next portion. Finally, the round bottom flask was rinsed with acetone and the resulting solid was combined with other portions. The solid was dried by passing nitrogen through the filtration bed overnight, giving 391 g (1.14 mol, 94%) of pale yellow hygroscopic powder. The 1H NMR showed that it contained residual sulfolane in a 0.023:1 mol ratio (Figure 1).[00032] Subsequent studies showed that less PBr3 is needed for this reaction, the 0.33:1 mol ratio required by the stoichiometry is nearly adequate and excess PBr3 contributes to the formation of colored impurities which are removed from the final product as described below. It was also found that the buildup of product cake after PBr3 addition can be prevented by increasing the initial sulfolane charge and by maintaining the reactor temperature at about 120C.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,4461-39-6, its application will become more common.

Reference:
Patent; ALBEMARLE CORPORATION; WO2007/53730; (2007); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Synthetic Route of 2807-30-9 ,Some common heterocyclic compound, 2807-30-9, molecular formula is C5H12O2, 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.

Examples 3 to 14 – synthesis of 2-amino-4-substituted-6-(4-fluorophenyl)-pyrido(3,2-d) pyrimidinesTo a solution of the 2-amino-4-thiomethyl-6-(4-fluorophenyl)-pyrido(3,2- d)pyrimidine of example 2 (56 mg) in a suitable alcohol (5 ml) was added a 2 M solution of lithium diisopropylamide (LDA) in tetrahydrofuran (1 ml). The reaction mixture was stirred at room temperature for 3 days. The excess alcohol was evaporated in vacuo and the crude residue was purified by preparative thin layer chromatography on silica using a mixture of toluene and acetonitrile as the mobile phase (in a volume ratio of 1 :1 ). If necessary a second purification was performed by HPLC on a C18-RP column (100 x30mm Gemini 5 mum) with a gradient of H2O, 0.05% TEA-acetonitrile. The resulting compounds were isolated in yields varying from 30 to 50%, depending on the alcohol used, and were characterized by their mass spectra MS as indicated below.2-amino-4-(2-propoxyethoxy)-6-(4-fluorophenyl)pyrido(3,2-d)pyrimidine (example 3) was obtained from 2-propoxyethanol; MS (m/z) : 343 ([M+H]+, 100).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,2807-30-9, its application will become more common.

Reference:
Patent; GILEAD SCIENCES, INC.; WO2008/77650; (2008); A1;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Application of 20017-67-8, Adding some certain compound to certain chemical reactions, such as: 20017-67-8, name is 3,3-Diphenyl-1-propanol,molecular formula is C15H16O, 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 20017-67-8.

Step l In a round bottom flask under a nitrogen atmosphere, 3,3-Diphenylpropan-l-ol (5.0Og, 23.6 mmol) and TEA (7.15g, 70.8 mmol) were dissolved in CHCl3 (75 mL, dry). The solution was cooled with an ice-salt bath to -15C. Methane sulphonylchloride (6.72g, 59.0 mmol) was added dropwise over a period of 10 min. The solution was gradually allowed to warm to O0C and stored in the fridge at 4C overnight. The yellow/orange solution was then quenched with ice-water (ca 150 mL) and the layers were separated. The water layer was washed with CH2Cl2 (2 * 75mL), and the combined organic layers were dried (MgSO4), filtered and concentrated in vacuo at 200C. This yielded an oil that solidified upon standing (8.16g). The solid was ground, triturated with petroleum ether (50 mL) and the solid was collected by filtration (7.9Og off-white solid).

According to the analysis of related databases, 20017-67-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; KING’S COLLEGE LONDON; WO2008/87421; (2008); A2;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts

Application 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.

General procedure: In the Schlenk reaction vessel,Methyltri n-octylphosphonium methyl carbonate([Me (n-octyl) 3P] + [OCO2Me]-,Charge the catalyst (C1a), 55.8 muL, 0.12 mmol),Methyl methacrylate (MMA, 4 mL) was added and stirred at room temperature for 1 to 2 minutes. Then, 3-methylbutane-1,3-diol (compound (3a), 21 3 muL, 2.0 mmol), internal standard substance (4,4′-di-tert-butylbiphenyl, 53.3 mg, 0.20 mmol), 1.0 g of dried powdery molecular sieves 5A (MS 5A) was added, and the mixture was stirred at room temperature (25 C.) for 3 hours to carry out an ester exchange reaction represented by the following formula. During the reaction, the progress of the reaction was confirmed by thin layer chromatography (TLC) as appropriate. The reaction mixture was passed through a celite pad to remove MS 5A, MMA was distilled off from the mixture under reduced pressure, and after concentration, the yield of the reaction product was measured by 1H NMR (internal standard method). The concentrate was subjected to silica gel column chromatography (n-hexane: ethyl acetate = 50: 1 to 10: 1) to isolate a carboxylic acid monoester (compound (4a)). The yield and yield of the reaction product are shown in Table 1. In the reaction system, the reaction between the catalyst (C1a) and the alcohol derived from the raw material (compound (3a)) causes Me (n-octyl) 3P] + [OR5]-as a catalytically active species.(Most R5 is 3-hydroxy-3-methylbutyl).

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; Nagoya University; Ishihara, Kazuaki; Hatano, Manabu; (20 pag.)JP2019/26618; (2019); A;,
Alcohol – Wikipedia,
Alcohols – Chemistry LibreTexts