Water → HCID 23507525, 화합물

HRID 1373121노트

반응식

HRID 1373121 반응식
[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][NH:5][S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7].[H-].[Na+].F[C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1.O>CN(C=O)C>[CH3:1][N:2]([CH3:15])[CH2:3][CH2:4][N:5]([C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1)[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:7])=[O:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 9590p-FluoronitrobenzeneHCID 24758Sodium hydrideHCID 2478570N-[2-(dimethylamino)ethyl]benzenesulfonamide

생성물 1

HCID 23507525HCID 23507525, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

6.8 g (29.8 mmol) of N-(2-dimethylamino-ethyl)-phenylsulphonamide are dissolved in 100 ml of DMF and combined with 1.3 g (30 mmol) of sodium hydride (55% in oil). The mixture is stirred for one hour at ambient temperature. Then 4.2 g (29.8 mmol) of 4-fluoro-nitrobenzene are added, and stirring is continued for another 16 hours. After the addition of 300 ml of water the mixture is extracted with ethyl acetate. The organic phase is washed with water, dried and evaporated down. The residue is acidified with 1 N hydrochloric acid and washed with ethyl acetate. The aqueous phase is then made basic again with sodium hydroxide solution and extracted with ethyl acetate. The organic phase is dried and evaporated down.

후처리

  1. stirringstirring
  2. waitis continued for another 16 hours
  3. extractionis extracted with ethyl acetate
  4. washThe organic phase is washed with water
  5. customdried
  6. customevaporated down
  7. washwashed with ethyl acetate
  8. extractionextracted with ethyl acetate
  9. customThe organic phase is dried
  10. customevaporated down

출처 및 근거

ORD 기록
ord-2c445b79523945e9829d8614a259dc6c
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07160901B2

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