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Water → 3'-(2-Dibenzylaminoacetyl)-4'-fluoromethanesulfonanilide

HRID 2379184
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HRID 2379184 반응식
Br[CH2:2][C:3]([C:5]1[CH:6]=[C:7]([CH:13]=[CH:14][C:15]=1[F:16])[NH:8][S:9]([CH3:12])(=[O:11])=[O:10])=[O:4].[CH2:17]([NH:24][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.O>CN(C)C=O>[CH2:25]([N:24]([CH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:2][C:3]([C:5]1[CH:6]=[C:7]([CH:13]=[CH:14][C:15]=1[F:16])[NH:8][S:9]([CH3:12])(=[O:11])=[O:10])=[O:4])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 7656DibenzylamineHCID 221413933'-(2-Bromoacetyl)-4'-fluoromethanesulfonanilide

생성물 1

HCID 189580893'-(2-Dibenzylaminoacetyl)-4'-fluoromethanesulfonanilide수율 84.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

3'-(2-Bromoacetyl)-4'-fluoromethanesulfonanilide (30 g) was dissolved in 200 ml of N,N-dimethylformamide, a solution of 38 g of dibenzylamine in N,N-dimethylformamide was added with ice-cooling and stirring and the mixture was made to react at room temperature for 1 hour. The reaction mixture was added to water followed by extracting with ethyl acetate. The extract was washed with water, dried, the solvent was evaporated therefrom and the residue was crystallized from diisopropyl ether to give 35 g of 3'-(2-dibenzylaminoacetyl)-4'-fluoromethanesulfonanilide. The crystals were made into hydrochloride to give 35 g of crystals, m.p. 185°-188° C.

후처리

  1. temperaturecooling
  2. customto react at room temperature for 1 hour
  3. extractionby extracting with ethyl acetate
  4. washThe extract was washed with water
  5. customdried
  6. customthe solvent was evaporated
  7. customthe residue was crystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-5a963038e9db42a18b8ec211a5c078ab
출처 데이터셋
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05360822

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