Water → t-Butyl N-(2-benzoylphenyl)-N-(p-toluenesulfonyl)aminoacetate

HRID 1871817

반응식

HRID 1871817 반응식
[C:1]1([CH3:25])[CH:6]=[CH:5][C:4]([S:7]([NH:10][C:11]2[CH:24]=[CH:23][CH:22]=[CH:21][C:12]=2[C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:14])(=[O:9])=[O:8])=[CH:3][CH:2]=1.[H-].[Na+].Br[CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31].O>CN(C)C=O>[C:13]([C:12]1[CH:21]=[CH:22][CH:23]=[CH:24][C:11]=1[N:10]([CH2:29][C:30]([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31])[S:7]([C:4]1[CH:3]=[CH:2][C:1]([CH3:25])=[CH:6][CH:5]=1)(=[O:9])=[O:8])(=[O:14])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 79177tert-Butyl bromoacetateHCID 233206N-(2-Benzoylphenyl)-4-methylbenzenesulfonamide

생성물 1

HCID 18688807t-Butyl N-(2-benzoylphenyl)-N-(p-toluenesulfonyl)aminoacetate수율 95.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a stirred solution of 5.0 g of compound H in 10 cc of dimethylformamide was added 0.56 g of 63% sodium hydride in 5 cc of dimethylformamide under ice-cooling and the mixture was stirred for 30 minutes. Then, 2.3 cc of t-butyl bromoacetate was added dropwise at the same temperature and stirring was continued for 16 hours. Water was added to the reaction mixture and the desired compound was extracted with ethyl acetate. The extract was washed with water and dried over magnesium sulfate. The solvent was distilled off and the crude product thus obtained was washed with hexane to obtain 6.31 g of compound I. Yield: 95.4%.

후처리

  1. temperaturecooling
  2. stirringstirring
  3. waitwas continued for 16 hours
  4. extractionthe desired compound was extracted with ethyl acetate
  5. washThe extract was washed with water
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent was distilled off
  8. customthe crude product thus obtained
  9. washwas washed with hexane

출처 및 근거

ORD 기록
ord-aa24dcc414ce4a0db5e75eb596a02395
출처 데이터셋
uspto-grants-2000_08
특허 번호
USRE036832

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