Potassium Iodide → HCID 20378254、化合物

HRID 2051952ノート

反応式

HRID 2051952 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 20378254HCID 20378254、化合物収率 63.9%

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 (0.012 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).

後処理

  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

出典と根拠

ORDレコード
ord-cc800ac9ec484a01bc50b9acde65b605
出典データセット
uspto-grants-1980_01
特許番号
US04182769

反応ノート

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