Chloroform → HCID 22397641, 화합물

HRID 1070759노트

반응식

HRID 1070759 반응식
[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

참가 물질

5

반응물 3

HCID 6212ChloroformHCID 154103-Chloropropanesulphonyl chlorideHCID 70048Benzhydrylpiperazine

생성물 1

HCID 22397641HCID 22397641, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b7fdd870f7a0494cb3cb2e2baa333cd5
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06903118B1

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