Downstream synthetic route of 74879-18-8

74879-18-8 (S)-(+)-2-Methylpiperazine 2734219, apiperazines compound, is more and more widely used in various fields.

74879-18-8, (S)-(+)-2-Methylpiperazine is a piperazines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,74879-18-8

Example 5 (0326) [0227] Compound 154 was prepared according to the reaction scheme in Figures 3 and 4. (0327) [0228] In a first step, compound 40 was prepared from compound 30 as follows: (0328) (0329) 30 40 (0330) [0229] Water (500 g, 5 w/w%) was charged to a reaction flask. Compound 30 (2- methylpiperazine) (100 g, 998.4 mmol, 1 eq.) was charged to the reaction flask with agitation. HC1 (36% aqueous, 102.1 g, 1008 mmol, 1.01 eq.) and methanol (200 g) were charged to the reaction flask with agitation. A solution of Boc20 (222 g, 1008 mmol, 1.01 eq.) in methanol (200 g) was added dropwise to the reaction flask at 15 to 25 C followed by stirring for 18 hours at 20 to 30C. The flask contents were evaporated to dryness in vacuo at 40 to 50C to form a residue. Water (500 g) was added to the residue and the mixture was stirred for 1 hours. The mixture was filtered and the collected solids were washed with water (50 g). The aqueous filtrate was extracted with ethylacetate (500 mL). The extracted aqueous phase was adjusted to a pH in excess of 12 with 30% NaOH and was then extracted with ethylacetate (500 mL) three times. The organic phase was washed with brine (500 g) twice and was then dried with anhydrous Na2S04. The dried mixture was filtered and the collected solids were rinsed with ethylacetate (100 mL). The filtrate was concentrated to dryness in vacuo at 50 to 60C and further concentrated under high vacuum (5 mm Hg) at 65 to 75C for 3 hours to yield compound 40 (tert-butyl 3-methylpiperazine-l-carboxylate). The purity of compound 40 was 97.7 area%, the assay was 95.9% and the yield was 76.4%.

74879-18-8 (S)-(+)-2-Methylpiperazine 2734219, apiperazines compound, is more and more widely used in various fields.

Reference£º
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; BEAUDRY, Danial; CRAVILLION, Theresa; GOSSELIN, Francis; LIM, Ngiap-Kie; MALHOTRA, Sushant; TIAN, Qingping; ZHANG, Haiming; GMEHLING, Alexander; FETTES, Alec; BACHMANN, Stephan; (130 pag.)WO2018/109050; (2018); A1;,
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