Dimethylformamide → 1-(4-Phenyl-4-phenylsulfonylbutyl)-4-phenylpiperazine oxalate

HRID 1112409노트

반응식

HRID 1112409 반응식
Cl[CH2:2][CH2:3][CH2:4][CH:5]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[S:6]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=[O:8])=[O:7].[C:21]1([N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[C:33](=[O:36])([O-:35])[O-].[Na+].[Na+].CN(C)[CH:41]=[O:42]>O>[C:41]([OH:42])(=[O:7])[C:33]([OH:35])=[O:36].[C:15]1([CH:5]([S:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)(=[O:8])=[O:7])[CH2:4][CH2:3][CH2:2][N:30]2[CH2:31][CH2:32][N:27]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:28][CH2:29]2)[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 70961-PhenylpiperazineHCID 10340Sodium CarbonateHCID 22763811[1-(Benzenesulfonyl)-4-chlorobutyl]benzene

생성물 1

HCID 227637831-(4-Phenyl-4-phenylsulfonylbutyl)-4-phenylpiperazine oxalate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 6.16 g of 1-chloro-4-phenyl-4-phenylsulfonylbutane, 4.25 g of 1-phenylpiperazine, 3.5 of sodium carbonate and 80 ml of dimethylformamide was refluxed with stirring for 23 hours. After cooling, water was added to the reaction mixture. The resulting mixture was extracted with chloroform, and the extract was washed with a 10% aqueous hydrochloric acid solution and with an aqueous potassium carbonate solution. To the organic layer was added 1.8 g of oxalic acid. The resulting oxalate was purified with 60% ethanol to give 6 g of 1-(4-phenyl-4-phenylsulfonylbutyl)-4-phenylpiperazine oxalate as white crystals, melting at 179°-181° C with decomposition.

후처리

  1. temperaturewas refluxed
  2. temperatureAfter cooling
  3. extractionThe resulting mixture was extracted with chloroform
  4. washthe extract was washed with a 10% aqueous hydrochloric acid solution and with an aqueous potassium carbonate solution
  5. additionTo the organic layer was added 1.8 g of oxalic acid
  6. customThe resulting oxalate was purified with 60% ethanol

출처 및 근거

ORD 기록
ord-048b3a994b2644e5ac44c1e92840d2a3
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04122178

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