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

HRID 1112409ノート

反応式

HRID 1112409 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-048b3a994b2644e5ac44c1e92840d2a3
出典データセット
uspto-grants-1978_10
特許番号
US04122178

反応ノート

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