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Potassium Carbonate → HCID 20378252, 화합물

HRID 2051943
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HRID 2051943 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[CH2:26][O:27][CH2:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:28]([O:27][CH2:26][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])[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 137983Benzyl chloromethyl ether2회HCID 135080754,5-Diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole

생성물 1

HCID 20378252HCID 20378252, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 3.5 g (0.01 mole) of 4,5-diphenyl-2-(1,1,2,2-tetrafluoroethylthio)imidazole, 2.1 g (0.013 mole) benzyl chloromethyl ether, 3.6 g (0.026 mole) potassium carbonate in 25 ml DMF was stirred for 24 hours. TLC showed some starting material, so an additional 0.5 g (0.003 mole) of benzyl chloromethyl ether was added and stirring continued for another 24 hours. The mixture was poured into ice water, extracted three times with ether and the ether layers backwashed three times with water. The ether solution was dried and concentrated on a rotary evaporator. The residue was chromatographed on 200 g SilicAR CC-7, eluting with toluene to give, after recrystallization from hexane, 3.6 g (76.6%) of white product, mp 70°-70.5°.

후처리

  1. stirringstirring
  2. waitcontinued for another 24 hours
  3. extractionextracted three times with ether
  4. dry with materialThe ether solution was dried
  5. concentrationconcentrated on a rotary evaporator
  6. customThe residue was chromatographed on 200 g SilicAR CC-7
  7. washeluting with toluene
  8. customto give
  9. customafter recrystallization from hexane, 3.6 g (76.6%) of white product, mp 70°-70.5°

출처 및 근거

ORD 기록
ord-18be0d29d43f4d2d96b1d0d4e16b15f8
출처 데이터셋
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04182769

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