Potassium Iodide → HCID 20378254, 화합물

HRID 2051952노트

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HRID 2051952 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([S:20]([C:23]([F:28])([F:27])[CH:24]([F:26])[F:25])(=[O:22])=[O:21])[NH:11][C:12]=2[C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.CC(C)([O-])C.[K+].[C:35]([O:41][CH2:42]Cl)(=[O:40])[C:36]([CH3:39])([CH3:38])[CH3:37].[I-].[K+]>C(COC)OC>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]=[C:10]([S:20]([C:23]([F:28])([F:27])[CH:24]([F:25])[F:26])(=[O:21])=[O:22])[N:11]([CH2:42][O:41][C:35](=[O:40])[C:36]([CH3:39])([CH3:38])[CH3:37])[C:12]=2[C:13]2[CH:14]=[CH:15][C:16]([F:19])=[CH:17][CH:18]=2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 44188TiflamizoleHCID 87885Chloromethyl pivalateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 20378254HCID 20378254, 화합물수율 63.9%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매2회

실험 절차

To a solution of 5.0 g (0.012 mole) of 4,5-bis(4-fluorophenyl)-2-(1,1,2,2-tetrafluoroethylsulfonyl)imidazole in 50 ml glyme was added 1.7 g (0.015 mole) of potassium t-butoxide, followed by a solution of 4.6 g (0.031 mole) of chloromethyl pivalate in 25 ml of glyme dropwise and a catalytic amount of potassium iodide. The reaction mixture was heated at reflux overnight, then poured onto water. The aqueous mixture was extracted with ether. The combined ether extracts were washed, then dried and concentrated to give 13.4 g of crude oily product. The product was purified by chromatography on silica gel, eluting with toluene, to give 4.1 g of crystals, mp 121°-123.5° (from methyl cyclohexane).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureat reflux overnight
  3. additionpoured onto water
  4. extractionThe aqueous mixture was extracted with ether
  5. washThe combined ether extracts were washed
  6. customdried
  7. concentrationconcentrated
  8. customto give 13.4 g of crude oily product
  9. customThe product was purified by chromatography on silica gel
  10. washeluting with toluene

출처 및 근거

ORD 기록
ord-cc800ac9ec484a01bc50b9acde65b605
출처 데이터셋
uspto-grants-1980_01
특허 번호
US04182769

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