{"id":1712,"date":"2021-02-09T05:19:50","date_gmt":"2021-02-08T21:19:50","guid":{"rendered":"https:\/\/www.pyrazoles-derivatives.com\/?p=1712"},"modified":"2021-02-09T05:19:50","modified_gmt":"2021-02-08T21:19:50","slug":"share-a-compound-402-61-9","status":"publish","type":"post","link":"https:\/\/www.pyrazoles-derivatives.com\/?p=1712","title":{"rendered":"Share a compound : 402-61-9"},"content":{"rendered":"<p><a href=\"https:\/\/www.ambeed.com\/products\/402-61-9.html\">Related Products of 402-61-9<\/a>, A common heterocyclic compound, 402-61-9, name is 5-Methyl-1H-pyrazole-3-carboxylic acid, molecular formula is C5H6N2O2, 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.<\/p>\n<p>Example 14; 5 -Methyl- lH-pyrazole-3-carboxylic acid [2-methyl-4-(2(2S)-methyl- [1 ,3&#8242;(3 &#8216; S)]bipyrrolidinyl- 1 &#8216;-yl)-phenyl] -amide; 2-Methyl-4-(2(2S)-methyl-[l,3&#8242;(3&#8217;S)]bipyrrolidinyl-r-yl)-phenylamine (330 mg, 1.15 mmol) was dissolved in DCM (6 mL) and DMF (2 mL), and the solution was cooled in an ice- water bath. To this solution was added powdered 5 -methyl- lH-pyrazole-3-carboxylic acid (174.6 mg, 1.38 mmol, 1.2 equiv.), N-methylmorpholine (280mg, 3 equiv.), 1- hydroxylbenzotriazole (HOBT) (0.162 g, 1.19 mmol, 1.3 equiv.), sequentially, and finally EDC HCl (0.228 g, 1.19 mmol, 1.3 equiv.). The resulting clear brown solution was stirred at r.t. overnight. TLC (10% MeOH in DCM) and LC\/MS showed that the reaction was complete and the product peak (368) was detected. The reaction was quenched with saturated sodium bicarbonate aqueous solution (3 mL) and 3 mL of DCM. The two layers were separated, and the aqueous layer was extracted with DCM (5 mLx2). The combined DCM extracts were washed with sodium bicarbonate (5mL) and brine (5 mL), dried (anhydrous potassium carbonate), filtered, and concentrated in vacuo to obtain a crude product which was purified <n=\"42\"\/>on a silica gel column (25 g of silica gel) on Analogix to obtain the title compound as a tan solid, 207 mg (49% yield).LCMS: Rx = 1.61 minutes, MS: 368 (M+H).1H NMR (300MHz, CDCl3), delta (ppm): 8.3 ((bs, IH), 7.65 (d, 9.6Hz, IH), 6.64 (s, IH), 6.43-6.39 (m, 2H), 3.52 (m, IH), 3.39 (m, IH), 3.26 (m, 2H), 3.02 (m, IH), 2.78 (m, IH), 2.53 (q,8.1Hz, IH), 2.37 (s, 3H), 2.28 (s, 3H), 2.12 (m, IH), 1.98 (m 2H), 1.78 (m, 2H), 1.51 (m, 2H).<\/p>\n<p>The synthetic route of 402-61-9 has been constantly updated, and we look forward to future research findings.<\/p>\n","protected":false},"excerpt":{"rendered":"<p>The synthetic route of 402-61-9 has been constantly updated, and we look forward to future research findings.<\/p>\n","protected":false},"author":8,"featured_media":0,"comment_status":"closed","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"footnotes":""},"categories":[159,131],"tags":[126],"class_list":["post-1712","post","type-post","status-publish","format-standard","hentry","category-402-61-9","category-pyrazoles-derivatives","tag-m-w100-200"],"yoast_head":"<!-- This site is optimized with the Yoast SEO plugin v24.9 - 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