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Benzenesulfonyl chloride → HCID 20378269, 화합물

HRID 2051953
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HRID 2051953 반응식
[C:1]1([C:7]2[N:8]=[C:9]([S:18][C:19]([F:24])([F:23])[CH:20]([F:22])[F:21])[NH:10][C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.CC(C)([O-])C.[K+].[C:31]1([S:37](Cl)(=[O:39])=[O:38])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1>C(COC)OC>[C:31]1([S:37]([N:10]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[N:8]=[C:9]2[S:18][C:19]([F:23])([F:24])[CH:20]([F:22])[F:21])(=[O:39])=[O:38])[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7369Benzenesulfonyl chlorideHCID 135080754,5-Diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazoleHCID 23665647Potassium tert-butoxide

생성물 1

HCID 20378269HCID 20378269, 화합물수율 125.9%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

To a stirred solution of 7.0 g (0.02 mole) of 4,5-diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole in 50 ml glyme at 0° was added 3.4 g (0.03 mole) of potassium t-butoxide. The mixture was stirred at 0° for five minutes, then a solution of 5.3 g (0.03 mole) of benzenesulfonyl chloride in 50 ml glyme was added dropwise. The mixture was stirred at 0° for one hour, then at room temperature overnight. The mixture was poured onto ice water and the crude solid product was collected and washed with water and hexane to give 12.4 g of tan solid. The product was purified by chromatography on silica gel, eluting with toluene, to give 7.2 g, white crystals, mp 171.5°-172.5° (from methylcyclohexane).

후처리

  1. stirringThe mixture was stirred at 0° for one hour
  2. customat room temperature
  3. customovernight
  4. additionThe mixture was poured onto ice water
  5. customthe crude solid product was collected
  6. washwashed with water and hexane

출처 및 근거

ORD 기록
ord-b0d8fd9111c9447fb1d266f7c1e1ac53
출처 데이터셋
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04182769

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