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Benzyl chloroformate → HCID 20378272, 화합물

HRID 2051951
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HRID 2051951 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+].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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10387Benzyl chloroformateHCID 135080754,5-Diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazoleHCID 23665647Potassium tert-butoxide

생성물 1

HCID 20378272HCID 20378272, 화합물수율 177.7%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-2224d295f8ec4ea4a05becdc7aa80e87
출처 데이터셋
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04182769

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