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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → HCID 20378262, 화합물

HRID 2051944
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HRID 2051944 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.Cl[C:26]([O:28][CH2:29][CH3:30])=[O:27].O.C(O)(=O)C>N1C=CC=CC=1>[C:12]1([C:11]2[N:10]=[C:9]([S:18][C:19]([F:23])([F:24])[CH:20]([F:22])[F:21])[N:8]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[C:7]=2[C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 10928Ethyl chloroformate2회HCID 135080754,5-Diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole

생성물 1

HCID 20378262HCID 20378262, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 1.76 g (5 mmole) 4,5-diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole, 1.1 g (10 mmole) of ethyl chloroformate in 10 ml pyridine was stirred at RT overnight. TLC showed some starting material, so another 0.6 g (5 mmole) of ethyl chloroformate was added and stirring was continued another 24 hours. The mixture was poured into water, neutralized with acetic acid and extracted three times with ether. The ether extracts were backwashed three times with water, then dried and concentrated. The last traces of pyridine were removed by pumping at 50° (0.5 mm). The residue was chromatographed on 150 g SilicAR CC-7, eluting with toluene to give, after recrystallization from hexane, 1.05 g (55%) of white product, mp 126.5°-127°.

후처리

  1. stirringstirring
  2. waitwas continued another 24 hours
  3. extractionextracted three times with ether
  4. customdried
  5. concentrationconcentrated
  6. customThe last traces of pyridine were removed
  7. customby pumping at 50°
  8. customThe residue was chromatographed on 150 g SilicAR CC-7
  9. washeluting with toluene
  10. customto give
  11. customafter recrystallization from hexane, 1.05 g (55%) of white product, mp 126.5°-127°

출처 및 근거

ORD 기록
ord-27335b0aca694a54a9fede996c0499f9
출처 데이터셋
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04182769

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