1,3-Dichloroacetone → 4-Chloromethyl-2-[2-(2-fluoro-4-trifluoromethyl-phenyl)-vinyl]-oxazole

HRID 1296548노트

반응식

HRID 1296548 반응식
[F:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[CH:4][C:3]=1[CH:12]=[CH:13][C:14]([NH2:16])=[O:15].[Cl:17][CH2:18][C:19]([CH2:21]Cl)=O>C1(C)C=CC=CC=1>[Cl:17][CH2:18][C:19]1[N:16]=[C:14]([CH:13]=[CH:12][C:3]2[CH:4]=[CH:5][C:6]([C:8]([F:11])([F:10])[F:9])=[CH:7][C:2]=2[F:1])[O:15][CH:21]=1

참가 물질

4

반응물 2

HCID 107931,3-DichloroacetoneHCID 691109983-(2-Fluoro-4-trifluoromethyl-phenyl)-acrylamide

생성물 1

HCID 690723654-Chloromethyl-2-[2-(2-fluoro-4-trifluoromethyl-phenyl)-vinyl]-oxazole수율 23%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

4.00 g (17.1 mmol) 3-(2-Fluoro-4-trifluoromethyl-phenyl)-acrylamide, 2.60 g (21.3 mmol) 1,3-dichloroacetone and 40 ml toluene were kept at reflux temperature for 16 h with continuous removal of water by use of a Dean-Stark trap. After cooling to room temperature, two extractions with 100 ml water, the organic phase was dried over sodium sulphate and the solvent removed in vacuo. Chromatography on silica gel (eluent: n-heptane/ethyl acetate 5:1) gave 1.20 g (23%) 4-chloromethyl-2-[2-(2-fluoro-4-trifluoromethyl-phenyl)-vinyl]-oxazole.

후처리

  1. temperatureat reflux temperature for 16 h
  2. customwith continuous removal of water by use of a Dean-Stark trap
  3. extractiontwo extractions with 100 ml water
  4. dry with materialthe organic phase was dried over sodium sulphate
  5. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-1cfc118b2707439f9b1bbec70e5c47f8
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07247649B2

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