Chloroform → HCID 22397641、化合物

HRID 1070759ノート

反応式

HRID 1070759 の反応式
[CH:1]([N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:20][CH2:21][CH2:22][CH2:23][S:24](Cl)(=[O:26])=[O:25].C(Cl)(Cl)Cl>ClCCl>[C:2]1([CH:1]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:14]2[CH2:19][CH2:18][N:17]([S:24]([CH2:23][CH2:22][CH2:21][Cl:20])(=[O:26])=[O:25])[CH2:16][CH2:15]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 6212ChloroformHCID 154103-Chloropropanesulphonyl chlorideHCID 70048Benzhydrylpiperazine

生成物 1

HCID 22397641HCID 22397641、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

39.2 g (155 mmol) benzhydrylpiperazine and 19.7 ml (141 mmol) TEA are present in 100 ml absolute dichloromethane and cooled to ca. 0° C. under moisture exclusion. 25 g (141 mmol) 3-chloropropanesulfonyl chloride are dissolved in 70 ml absolute dichloromethane and added dropwise. The mixture is stirred for two hours under cooling and subsequently mixed with chloroform and washed with saturated NaCl solution. The organic phase is dried over sodium sulfate and concentrated under vacuum until dry. The solid is further processed without further purification: yield 59.2 g.

後処理

  1. additionadded dropwise
  2. temperatureunder cooling
  3. washwashed with saturated NaCl solution
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. concentrationconcentrated under vacuum
  6. customuntil dry
  7. customThe solid is further processed without further purification

出典と根拠

ORDレコード
ord-b7fdd870f7a0494cb3cb2e2baa333cd5
出典データセット
uspto-grants-2005_06
特許番号
US06903118B1

反応ノート

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