N-bromobutanimide → HCID 68428209, 화합물

HRID 642333노트

반응식

HRID 642333 반응식
[CH2:1]([O:3][C:4]([C:6]1[S:10][C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:13][CH:12]=2)=[N:8][C:7]=1[CH3:24])=[O:5])[CH3:2].[Br:25]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[CH2:1]([O:3][C:4]([C:6]1[S:10][C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)=[CH:13][CH:12]=2)=[N:8][C:7]=1[CH2:24][Br:25])=[O:5])[CH3:2]

참가 물질

5

반응물 2

HCID 67184N-bromobutanimideHCID 684263914-Methyl-2-(4-phenoxy-phenyl)-thiazole-5-carboxylic acid ethyl ester

생성물 1

HCID 68428209HCID 68428209, 화합물수율 97.6%

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 5943Carbon Tetrachloride용매

실험 절차

A mixture of 4-methyl-2-(4-phenoxy-phenyl)-thiazole-5-carboxylic acid ethyl ester (1.40 g, 4.14 mmole), N-bromosuccinimide (760 mg, 4.27 mole) and benzoyl peroxide (50 mg, 0.21 mmole) in carbon tetrachloride (18 ml) was refluxed for 8 h before it was cooled to room temperature and partitioned between dichloromethane and water. The organic layer was washed with saturated aqueous sodium bicarbonate solution, brine, dried over anhydrous sodium sulfate and concentrated in vacuo to give the title compound as a yellow oil (1.69 g). MS: (+) m/z 417.87, 419.87 (M+1, 79Br/81Br).

후처리

  1. temperaturewas refluxed for 8 h before it
  2. custompartitioned between dichloromethane and water
  3. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution, brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-2a5345111e1a4d478a4e24fdee23da4a
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07696223B2

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