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Chlorosulfonic acid → HCID 11178065, 화합물

HRID 1266149
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HRID 1266149 반응식
[Cl:1][C:2]([Cl:20])([Cl:19])[C:3]([N:5]1[CH2:10][CH2:9][N:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[O:17][CH3:18])[CH2:7][CH2:6]1)=[O:4].[Cl:21][S:22](O)(=[O:24])=[O:23]>ClCCl>[Cl:20][C:2]([Cl:1])([Cl:19])[C:3]([N:5]1[CH2:6][CH2:7][N:8]([C:11]2[CH:16]=[C:15]([S:22]([Cl:21])(=[O:24])=[O:23])[CH:14]=[CH:13][C:12]=2[O:17][CH3:18])[CH2:9][CH2:10]1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24638Chlorosulfonic acidHCID 33831142-(4-Trichloroacetylpiperazin-1-yl) anisole

생성물 1

HCID 11178065HCID 11178065, 화합물수율 46%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 2-(4-trichloroacetylpiperazin-1-yl) anisole (D1) (10 g) in dichloromethane (115 ml) was added over 0.3 h to ice-cooled chlorosulfonic acid (52 ml). After 0.5 h at 0° C. then 1 hour at ambient temperature, the solution was poured onto a mixture of ice-water (500 g) and dichloromethane (500 ml) with rapid stirring. The layers were separated and the organic phase was washed with water (2×800 ml), dried (MgSO4) and concentrated to give the title compound (D2) as a foam (6.0 g, 46%), MH+ 435/437.

후처리

  1. customThe layers were separated
  2. washthe organic phase was washed with water (2×800 ml)
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4229bff10c0542aab84376550b347eb4
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06548504B1

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