m-Chloroperbenzoic acid → N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide

HRID 23388

반응식

HRID 23388 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][S:9][CH3:10])[C:3]=1[NH:11][C:12](=[O:17])[C:13]([F:16])([F:15])[F:14].ClC1C=C(C=CC=1)C(OO)=O.[O-2:29].[Al+3].[O-2:31].[O-2].[Al+3]>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH2:8][S:9]([CH3:10])(=[O:31])=[O:29])[C:3]=1[NH:11][C:12](=[O:17])[C:13]([F:15])([F:16])[F:14]

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acidHCID 9989226AluminaHCID 22574009N-(2-Chloro-6-methylsulfanylmethyl-phenyl)-2,2,2-trifluoro-acetamide

생성물 1

HCID 22574080N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The crude solid N-(2-chloro-6-methylsulfanylmethyl-phenyl)-2,2,2-trifluoro-acetamide from Step 2 was redissolved in methylene chloride (300 ml) and treated at 0° C. with meta-chloroperoxybenzoic acid (39.88 g, 0.177 mole) in portions with stirring. After 90 minutes the entire reaction mixture was poured onto a column of deactivated aluminum oxide (6% water) and the product was washed free of the acid by eluting with 1:1 ethyl acetate:hexane to afford 22.28 g of N-(2-Chloro-6-methanesulfonylmethyl-phenyl)-2,2,2-trifluoro-acetamide, a crystalline product (86%).

후처리

  1. customAfter 90 minutes the entire reaction mixture
  2. washthe product was washed free of the acid
  3. washby eluting with 1:1 ethyl acetate

출처 및 근거

ORD 기록
ord-52c4651d64e1430795428fe882f2b19a
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852726B2

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