Potassium Carbonate → 1-Benzyl-4-[(5-chloroisoindol-2-yl)sulfonyl]piperazine

HRID 352778ノート

反応式

HRID 352778 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][N:11]([S:14](=[O:17])(=[O:16])[NH2:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[CH2:19][C:20]1[CH:21]=[C:22]([Cl:28])[CH:23]=[CH:24][C:25]=1[CH2:26]Br.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH2:1]([N:8]1[CH2:9][CH2:10][N:11]([S:14]([N:15]2[CH:19]=[C:20]3[C:25]([CH:24]=[CH:23][C:22]([Cl:28])=[CH:21]3)=[CH:26]2)(=[O:17])=[O:16])[CH2:12][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 112305864-Benzylpiperazine-1-sulfonamideHCID 150082261,2-Bis(bromomethyl)-4-chlorobenzene

生成物 1

HCID 227101621-Benzyl-4-[(5-chloroisoindol-2-yl)sulfonyl]piperazine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In ethanol (5 ml), 1-benzyl-4-sulfamoylpiperazine (251 mg) was dissolved. To the resulting solution, 3,4-bis(bromomethyl)-1-chlorobenzene (293 mg) and potassium carbonate (204 mg) were added, followed by heating under reflux for 3.5 hours. After cooling, the precipitate was filtered off. The filtrate was then distilled under reduced pressure and the residue was purified by chromatography on a silica gel column (dichloromethane˜ethanol:dichloromethane=1:100), whereby the title compound (222 mg, 58%) was obtained.

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 3.5 hours
  3. temperatureAfter cooling
  4. filtrationthe precipitate was filtered off
  5. distillationThe filtrate was then distilled under reduced pressure
  6. customthe residue was purified by chromatography on a silica gel column (dichloromethane˜ethanol:dichloromethane=1:100), whereby the title compound (222 mg, 58%)
  7. customwas obtained

出典と根拠

ORDレコード
ord-27d20b4baceb48d0b7bfa6089b63ecb4
出典データセット
uspto-grants-2004_06
特許番号
US06747023B1

反応ノート

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