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Benzyl chloroformate → HCID 20378272、化合物

HRID 2051951
ノート
印刷プレビュー

反応式

HRID 2051951 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+].Cl[C:32]([O:34][CH2:35][C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=1)=[O:33]>C(COC)OC>[CH2:35]([O:34][C:32]([N:10]1[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[N:8]=[C:9]1[S:18][C:19]([F:23])([F:24])[CH:20]([F:22])[F:21])=[O:33])[C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=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 10387Benzyl chloroformateHCID 135080754,5-Diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazoleHCID 23665647Potassium tert-butoxide

生成物 1

HCID 20378272HCID 20378272、化合物収率 177.7%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

To a solution of 5.0 g (0.014 mole) of 4,5-diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole in 50 ml glyme was added 1.7 g (0.015 mole) of potassium t-butoxide. The mixture was cooled and a solution of 5.0 g (0.029 mole) of benzyl chloroformate in 25 ml glyme was added dropwise. The reaction mixture was stirred at room temperature overnight, then poured onto water. The mixture was extracted with ether and the combined ether extracts were washed, then dried and concentrated to give 12.1 g of crystals. The product was purified by chromatography on silica gel, eluting with toluene, to give 2.1 g of colorless crystals (from hexane), mp 110°-111°.

後処理

  1. temperatureThe mixture was cooled
  2. additionpoured onto water
  3. extractionThe mixture was extracted with ether
  4. washthe combined ether extracts were washed
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-2224d295f8ec4ea4a05becdc7aa80e87
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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