Month: July 2021

Electric Literature of 637031-88-0 , The common heterocyclic compound, 637031-88-0, name is 3,3-Difluorocyclobutanol, molecular formula is C4H6F2O, 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 slurry of Intermediate 100 (40 mg, 0.085 mmol), 3,3-difluorocyclobutanol (11.5 mg,106 rnmoi), (4,4-di-t-butyi-2,2-bipyridine)bis[3,5-difluoro-2-[5-trifluoromethyi-2-pyridinyi- kappaN)phenyl-kappaCjiridium(lli) hexatluorophosphate (087 mg, 0.85 Itmol), nickei(ll) bromide ethylene glycol dimethyl ether complex (1.3 mg, 4.3 jimol), 4,4-di-tert-butyl-2,2- hipyridine (1.1 mg, 4.3 imol), potassium carbonate (14.7 mg, 0.106 mmol) and quinuclidine (0.95 mg, 8.50 jirnol) in CH3CN (850 il) was degassed, blanketed under N2 and irradiated with blue LED for 16 h, Additional amounts of 3-difluorocyclobutanol (11.5 mg, 0.106 mmoi), (4,4- di-t-butyi-2,2-bipyridine)bi s[3 , 5-difiuoro-2–[5-trifiuoromethyi-2-pyridinyl-kappan)phenyl kappaciiridiurn(1II) hexafluorophosphate (0.87 mg, 0.850 lrnol), nickei(II) bromide ethyleneglycol dimethyl ether complex (1.3 mg, 4.25 jimol), (1.1 mg,4.25 umol), potassium carbonate (14.7mg, 0.106 mrnoi) and quinuclidine (0.95 mg, 8.50 FIrnol) were added, the reaction mixture was degassed, blanketed under N2 and irradiated with blue LED for additional 16 h w/ air cooling. The reaction mixture was quenched with TFA, concentrated, suspended in DMF, filtered and purified by reverse phase HPLC to afford Example 360 (4.3 mg,10 % yield). MS ES1) ith: 497.9 (M+H). iHri4R (500 MHz, DMSO-d6) oe ppm ). 28 (br d,J=7.6 Hz, IH), 8.48 (br d, J7.6 Hz, 1H), 8.31 8.24 (rn, IH), 8.21 (s, IH), 8.16 (dd, J=7.5, 1.7Hz. HI), 7.69 (hr s, 1H), 7.59 (hr s, IH), 710 (dd, J=7.3, 5.2 Hz. 1EI), 6.99 (hr s, 1H), 6.82 (bid,J=7.3 Hz, IH), 5.23 (quin, J=7.2 Hz, IH), 4.90 (hr s, III), 4.43 .- 4.31 (rn, 1H), 3.28 (hr d, J=4.6Hz, IH), 281 – 270 (m, 2F), 2.70 2.59 (m, IH), 239 – 2.32 (in, 1H). 2.27 (hr dd, J1 1.3, 7.3Hz, IH), 2.21 (br d, J=4.0 Hz, 1H), 2.20 2.12 (m, 2H). Analytical HPLC RI? = 1.240 mm(Method A) and 1.554 mm (Method B), purity 95%.

The synthetic route of 637031-88-0 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; SMITH II, Leon M.; LADZIATA, Vladimir; DELUCCA, Indawati; PINTO, Donald, J., P.; ORWAT, Michael J.; DILGER, Andrew K.; PABBISETTY, Kumar Balashanmuga; YANG, Wu; SHAW, Scott A.; GLUNZ, Peter W.; PANDA, Manoranjan; (612 pag.)WO2017/123860; (2017); A1;,
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Related Products of 29171-20-8, 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 29171-20-8, name is 3,7-Dimethyloct-6-en-1-yn-3-ol. This compound has unique chemical properties. The synthetic route is as follows.

In the air, a sulfonic acid resin T239 (2.31 g) was added to a 500 mL autoclave at room temperature, and the autoclave was sealed.The air in the autoclave was replaced with nitrogen three times, and finally the nitrogen pressure in the autoclave was maintained at 2.0 MPa.Dehydrogenated linalool (76.89 g, 0.5 mol) and 2-methoxypropene (109.25 g, 1.5 mol) were sequentially charged into the autoclave by a parallel flow pump.Turn on the autoclave stirring (300 rpm) and the heat tracing. When the internal temperature of the reactor reaches 90 ° C,Start timing, heat preservation reaction for 8 hours, sampling analysis, GC detection, complete conversion of the raw material dehydrogenated linalool.After the treatment, the reaction solution was cooled to room temperature, and the resin catalyst and the reaction liquid were separated by filtration through a sand core funnel, and the filtrate was subjected to rotary evaporation.Excess 2-methoxypropene and by-product methanol were removed to obtain 95.95 g of a enedoketone product with a purity of 98percent and a yield of 97.8percent.

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 29171-20-8, 3,7-Dimethyloct-6-en-1-yn-3-ol.

Reference:
Patent; Wanhua Chemical Group Co., Ltd.; Xie Shuo; Huang Wenxue; Wang Yanbin; (10 pag.)CN109534977; (2019); 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. 5259-98-3, name is 5-Chloropentan-1-ol. This compound has unique chemical properties. The synthetic route is as follows. Application In Synthesis of 5-Chloropentan-1-ol

General procedure: A solution of phthalimide (14.7 g, 0.1 mol) and 5-chloropentanol (11.25 g, 0.1 mol) or6-chloro-hexanol (12.45 g, 0.1 mol) in anhydrous DMF (100 mL) was heated at 150 °C with vigorousstirring in the presence of finely-powdered anhydrous K2CO3 (13.8 g, 0.1 mol) for 12 h. After cooling,the inorganic materials were filtered off and the solvent was evaporated in vacuo (2 mmHg, 100 °C).The residue was dissolved in 150 mL of ethyl acetate, and after standing overnight at 5 °C, the solutionwas filtered and concentrated in vacuo. The residue was taken up in 80 mL of CHCl3. After extractionwith 60 mL of 5percent aqueous solution of NaHCO3 and 3 60 mL of H2O, the solvent was dried overNa2SO4 and removed in vacuo, giving: 2-(5-Hydroxypentyl)-1H-isoindole-1,3(2H)-dione (5a). A sticky oil (on standing for a prolonged period theviscous oil crystallized giving a solid), yield 70percent (16.32 g); m.p. 41?43 °C; Rf = 0.39 (CHCl3/CH3OH20:1); 1H-NMR (300 MHz, CDCl3): delta= 1.40?1.43 (m, 4H, CH2C), 1.53?1.58 (m, CH2CH2OH), 1.66?1.71(m, 3H, CH2CH2N, OH), 3.61?3.63 (t, J = 6.6 Hz, 2H, CH2N), 3.66?3.68 (t, J = 7.2 Hz, 2H, CH2OH),7.68?7.71 (m, 2H, Harom); 7.81?7.84 (m, 2H, H) ppm.

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, 5259-98-3, 5-Chloropentan-1-ol.

Reference:
Article; Guryn, Roman; Staszewski, Marek; Stasiak, Anna; Flores, Daniel McNaught; Fogel, Wies?awa Agnieszka; Leurs, Rob; Walczynski, Krzysztof; Molecules; vol. 23; 2; (2018);,
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Electric Literature of 2215-78-3, 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. 2215-78-3, name is (4-Phenoxyphenyl)methanol, molecular formula is C13H12O2, 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.

4-Phenoxybenzyl alcohol (20.0 g) was dissolved in toluene (100 mL), and thionyl chloride (13.1 g) was added to the solution over 30 minutes at room temperature. After 2 hours, the reaction solution was concentrated under reduced pressure. The residue was distilled to give 16.7 g (yield: 76%) of the target product. A boiling point thereof was 137 C/3 mmHg.

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 2215-78-3, (4-Phenoxyphenyl)methanol.

Reference:
Patent; Agro Kanesho Co Ltd; Aizawa, Ryo; Okada, Itaru; (13 pag.)KR2016/85330; (2016); A;,
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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.105-30-6, name is 2-Methylpentan-1-ol, molecular formula is C6H14O, molecular weight is 102.18, as common compound, the synthetic route is as follows.Application In Synthesis of 2-Methylpentan-1-ol

(R)-methyl 2-(ter?-butoxycarbonylamino)-2-(4-hydroxyphenyl)acetate (23.00 g, 82 mmol), 2-methylpentan-l-ol (16.70 g, 163 mmol), and triphenylphosphine (36.46 g, 139 mmol) were combined in tetrahydrofuran (600 mL). After stirring 10 min, diethylazodicarboxylate (21.9 mL, 138 mmol) was added via syringe at room temperature. The reaction was mildly exothermic resulting in the temperature rising to the mid thirties C during the addition. Intermittent cooling with a tap water bath was used to prevent the reaction mixture temperature from rising higher than this, but it was not cooled down to room temperature during the addition. After the addition was complete, the mixture was stirred at room temperature for 18 h. The reaction mixture was transferred to a separatory funnel containing water (400 mL). The aqueous layer was extracted with ether (3 x 400 mL). The combined organic layers were washed with brine (250 mL), dried over MgS04, filtered and concentrated. The crude product was taken up in ether (ca. 800 mL) and was stirred for 30 min. The mixture was filtered through a pad of diatomaceous earth (Celite) to remove most of the triphenylphosphine oxide and the filtrate was concentrated. The residue was purified by column chromatography on silica gel (20% ethyl acetate in hexanes) to afford (2R)-methyl 2-(tert-butoxycarbonylamino)-2-(4-(2- methylpentyloxy)phenyl)acetate (29.43 g, 98% yield) as a colorless oil: XH NMR (400 MHz, CDC13) delta 7.20-7.29 (m, 2 H), 6.84 (d, J= 8.6 Hz, 2 H), 5.45 (d, J= 6.5 Hz, 1 H), 5.22 (d, J= 7.3 Hz, 1 H), 3.77 (dd, J= 9.1, 5.8 Hz, 1 H), 3.69 (s, 3 H),3.65-3.70 (m, 1 H), 1.85-1.96 (m, 1 H), 1.41 (s, 9 H), 1.14-1.50 (m, 4 H), 0.98 (d, J = 6.8 Hz, 3 H), 0.90 (t, J= 7.1 Hz, 3 H); LRMS (ESI) mle 366.4 [(M + H)+, calcd for C20H32NO5366.2].

At the same time, in my other blogs, there are other synthetic methods of this type of compound,105-30-6, 2-Methylpentan-1-ol, and friends who are interested can also refer to it.

Reference:
Patent; BRISTOL-MYERS SQUIBB COMPANY; LEXICON PHARMACEUTICALS, INC.; DZIERBA, Carolyn, Diane; HARTZ, Richard, A.; BI, Yingzhi; AHUJA, Vijay T.; BRONSON, Joanne J.; CARSON, Kenneth; CIANCHETTA, Giovanni; GREEN, Michael; KIMBALL, David; KIMURA, S. Roy; KWON, Soojin; MACOR, John E.; ZHANG, Yulian; ZIPP, Greg; WO2011/44225; (2011); A1;,
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In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 534-03-2, name is 2-Aminopropane-1,3-diol, the common compound, a new synthetic route is introduced below. Quality Control of 2-Aminopropane-1,3-diol

0.91 g of 2-amino-l , 3-propandiol and 1.13 g of triethylamine are solubilised in 15 ml of tetrahydrofuran at 0C. The solution is stirred and placed under nitrogen atmosphere. A solution of 2.74 g of palmitoyl chloride is added dropwise slowly within 30 min. After another 30 min of stirring at ambient temperature, the mixture is dry evaporated. The residue is solubilised using 15 ml of ethyl acetate and extracted using 10 ml of water which is disposed. The organic phase is anhydrified using Na2S04 and dry evaporated under vacuum. The raw amide thus obtained is used without further purification. The residue is suspended at 0C and under nitrogen gas atmosphere in 20 ml of S0C12. The mixture is stirred at 0C for 30 minutes, then at ambient temperature for 6 hours. The solution thus obtained is dry evaporated at a low pressure. The residue is purified by crystallization from 15 ml of tert-butyl methyl ether, isolated and dried under vacuum. The crystallized product is suspended in 20 ml of anhydrous toluene and 1.3 g of potassium tert- butoxide are added. The mixture is heated at 40C for 2 hours, then it is cooled at 4C. The solution is extracted 3 times using 6 ml of water and the extracts are disposed. The organic phase is dry evaporated at’ a low pressure and the residue purified through flash chromatography in a column of silica gel using – as eluent – a mixture of hexane and ethyl acetate 1:3. The fractions containing the pure product are recombined and dry evaporated under vacuum. (About 90% yield) The 2-pentadecyl-4-hydroxymethyl-2-oxazoline product has the following characteristics: Molecular formula C19H37N02; C=73.26%, H=11.97%, N=4.50%, 0=10.27%; Solubility: poorly soluble in water, >10 mg/ml in ethanol; Mr 311.5; ESI-MS: 312 (MH+) .

The synthetic route of 534-03-2 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; EPITECH GROUP S.r.L.; DELLA VALLE, Francesco; DELLA VALLE maria Federica; DI MARZO, Vincenzo; CUZZOCREA, Salvatore; WO2013/121449; (2013); A1;,
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