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Benzenesulfonyl chloride → HCID 20378269、化合物

HRID 2051953
ノート
印刷プレビュー

反応式

HRID 2051953 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 20378269HCID 20378269、化合物収率 125.9%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b0d8fd9111c9447fb1d266f7c1e1ac53
出典データセット
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04182769

反応ノート

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