1-Methylpiperazine → Benzonitrile, 2-fluoro-6-(4-methyl-1-piperazinyl)-

반응식

F[C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([F:10])[C:3]=1[C:4]#[N:5].[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>>[F:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([N:15]2[CH2:16][CH2:17][N:12]([CH3:11])[CH2:13][CH2:14]2)[C:3]=1[C:4]#[N:5]

참가 물질

반응물 2

HCID 531671-Methylpiperazine

HCID 746952,6-Difluorobenzonitrile

생성물 1

HCID 13469798Benzonitrile, 2-fluoro-6-(4-methyl-1-piperazinyl)-

실험 절차

2,6-Difluorobenzonitrile is reacted with N-methyl piperazine following the procedure of Example 5. The reaction mixture is extracted with methylene chloride after addition of water. The methylene chloride is extracted with dilute HCl which is basified and extracted with methylene chloride. The resulting crude oil after evaporation is taken in ethanol and i-PrOH-HCl is added to give the title compound as the hydrochloride salt, 1.4 g m.p. 245°-247° C.

후처리

extractionThe reaction mixture is extracted with methylene chloride
additionafter addition of water
extractionThe methylene chloride is extracted with dilute HCl which
extractionextracted with methylene chloride
customThe resulting crude oil after evaporation
additioni-PrOH-HCl is added

출처 및 근거

ORD 기록: ord-36441a7207f94b70bfa19aaa507cb8ea
출처 데이터셋: uspto-grants-1985_03
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04504660

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