Water → HCID 23507525、化合物

HRID 1373121ノート

反応式

HRID 1373121 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 23507525HCID 23507525、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2c445b79523945e9829d8614a259dc6c
出典データセット
uspto-grants-2007_01
特許番号
US07160901B2

反応ノート

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