Phosphorus oxychloride → 2-Chloro-8-(trifluoromethyl)quinoline

반응식

[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[NH:11][C:10](=O)[CH:9]=[CH:8]2.O=P(Cl)(Cl)[Cl:18]>>[Cl:18][C:10]1[CH:9]=[CH:8][C:7]2[C:12](=[C:3]([C:2]([F:15])([F:14])[F:1])[CH:4]=[CH:5][CH:6]=2)[N:11]=1

참가 물질

반응물 2

HCID 24813Phosphorus oxychloride

HCID 248957428-(Trifluoromethyl)quinolin-2(1H)-one

생성물 1

HCID 337782222-Chloro-8-(trifluoromethyl)quinoline수율 33%

실험 절차

8-Trifluoromethyl-1H-quinolin-2-one (8.35 g, 39.2 mmol) was taken in a 25 mL RB POCl3 (10 mL) was added, and then refluxed for 1 h. The excess POCl3 was distilled off and ice was added to the reaction mixture. This was stirred for 15 min, the precipitate was filtered off and then dried under vacuum to afford the title compound (3 g, yield: 33%).

후처리

additionwas added
temperaturerefluxed for 1 h
distillationThe excess POCl3 was distilled off
additionice was added to the reaction mixture
filtrationthe precipitate was filtered off
customdried under vacuum

출처 및 근거

ORD 기록: ord-ced68df90c104877ac009b731c0b2942
출처 데이터셋: uspto-grants-2013_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08604055B2

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