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[urri]

Добрый день!
Посмотрите,пожалуйста,получение
ClCC(=O)c1nc2ccccc2[nH]1
Спасибо!

[mishka]

получения нет
упоминается только реакция с (2-chloro-3-methoxyphenyl)-[3-(hydroxymethyl)piperazin-1-yl]methanone

With N-ethyl-N,N-diisopropylamine In tetrahydrofuran at 70℃; Inert atmosphere; Cooling with ice;


Current Patent Assignee: HOFFMANN LA ROCHE - WO2021/5034, 2021, A1
Location in patent: Page/Page column 94; 157
Experimental Procedure
60; 61 (2-chloro-3-methoxy-phenyl)-[rel-(3S,9aS)-3-(lH-benzimidazol-2-yl)-3-hydroxy- l,4,6,7,9,9a-hexahydropyrazino[2,l-c][l,4]oxazin-8-yl]methanone and (2-chloro-3- methoxy-phenyl)-[rel-(3R,9aR)-3-(lH-benzimidazol-2-yl)-3-hydroxy-l,4,6,7,9,9a- hexahydropyrazino[2, 1 -c] [ 1 ,4] oxazin-8-yl]methanone
(2-chloro-3 -methoxyphenyl)(3 -(hydroxymethyl)piperazin- 1 -yl)methanone (intermediate 1, 96 mg, 337 umol) and DIPEA (65 uL, 371 umol) were dispersed in 2 mL dry THF and cooled down in an ice bath. l-(lH-benzoΔimidazol-2-yl)-2-chloroethan-l-one (79 mg, 405 umol) was dissolved in 1 mL dry THF and added dropwise to the solution over 10 min. It was then heated up to 70°C overnight. It was concentrated in vacuo and then purified by silica column chromatography (DCM:MeOH 100:0 to 90: 10). The compound was obtained as a yellow solid (47 mg, 24%), the two enantiomers were separated by chiral SFC (method D). Example 60 (enantiomer A) 10.9 mg, ESI(MS) m/z = 443.2 [M+H]+ Example 61 (enantiomer B) 16.2 mg, ESI(MS) m/z = 443.2 [M+H]+

[urri]

Спасибо!