N-bromobutanimide → HCID 86655151, 화합물

HRID 69399노트

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HRID 69399 반응식
[CH2:1]([NH:5][C:6](=[O:31])[C:7]1[CH:12]=[CH:11][C:10]([C:13](=[N:28][OH:29])[CH:14]=[C:15]([C:20]2[CH:25]=[C:24]([Cl:26])[CH:23]=[C:22]([Cl:27])[CH:21]=2)[C:16]([F:19])([F:18])[F:17])=[CH:9][C:8]=1[CH3:30])[CH2:2][CH2:3][CH3:4].[Br:32]N1C(=O)CCC1=O>CN(C)C=O>[Br:32][CH:14]1[C:15]([C:20]2[CH:25]=[C:24]([Cl:26])[CH:23]=[C:22]([Cl:27])[CH:21]=2)([C:16]([F:18])([F:17])[F:19])[O:29][N:28]=[C:13]1[C:10]1[CH:11]=[CH:12][C:7]([C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])=[O:31])=[C:8]([CH3:30])[CH:9]=1

참가 물질

4

반응물 2

HCID 67184N-bromobutanimideHCID 76765796HCID 76765796, 화합물

생성물 1

HCID 86655151HCID 86655151, 화합물수율 40%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

N-Butyl-4-[3-(3,5-dichloro-phenyl)-4,4,4-trifluoro-1-hydroxyimino-but-2-enyl]-2-methyl-benzamide (Example 3.1) (380 mg, 0.94 mmol) and N-bromosuccinimide (200 mg, 1.12 mmol) were heated in N,N-dimethylformamide (2 ml) at 120° C. for 7 minutes. The reaction mixture was allowed to cool to ambient temperature and then extracted with diethyl ether. The combined organic extracts were dried over magnesium sulfate and concentrated. The residue was purified by chromatography on silica gel (eluent: hexane/ethyl acetate 4:1) to give Compound No. A1 of Table A (210 mg, 40% yield) as a solid foam.

후처리

  1. extractionextracted with diethyl ether
  2. dry with materialThe combined organic extracts were dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThe residue was purified by chromatography on silica gel (eluent: hexane/ethyl acetate 4:1)
  5. customto give Compound No

출처 및 근거

ORD 기록
ord-37ec0dd68a264f2caf7ebd0c6123e459
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822502B2

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