Ethanol → Ethyl 2-iodotetrafluoropropionate

HRID 963584

反応式

HRID 963584 の反応式
[F-].[K+].[CH2:3]([OH:5])[CH3:4].S(F)([O:9][C:10](F)(F)[C:11]([F:17])([I:16])[C:12]([F:15])([F:14])[F:13])(=O)=O>O>[I:16][C:11]([F:17])([C:12]([F:15])([F:14])[F:13])[C:10]([O:5][CH2:3][CH3:4])=[O:9]

参加物

5

反応物 3

HCID 702EthanolHCID 522689Potassium FluorideHCID 125963661,1,2,3,3,3-Hexafluoro-2-iodopropyl sulfurofluoridate

生成物 1

HCID 12119967Ethyl 2-iodotetrafluoropropionate収率 56%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
70 °C

実験手順

A 500 mL flask was charged with potassium fluoride (17.5 g, 0.31 mol) and absolute ethanol (110 mL), and was cooled in an ice-water bath. 2-iodo-hexafluoropropyl fluorosulfate (112.8 g, 0.3 mol) was added slowly. The reaction was exothermic and the reaction temperature was controlled at 20°-25° C. After addition was complete, the reaction mixture was heated at 70° C. for 4 hr and then poured into cold water. The bottom organic layer was separated, washed with saturated NaCl aqueous solution and dried over MgSO4. Evaporation of the solvent in vacuo followed by distillation gave 50 g (56% yield) of ethyl 2-iodotetrafluoropropionate product, formula above, having a boiling point of 60°-65° C. at 50 mmHg.

後処理

  1. temperaturewas cooled in an ice-water bath
  2. customwas controlled at 20°-25° C
  3. additionAfter addition
  4. customThe bottom organic layer was separated
  5. washwashed with saturated NaCl aqueous solution
  6. dry with materialdried over MgSO4
  7. customEvaporation of the solvent in vacuo
  8. distillationfollowed by distillation

出典と根拠

ORDレコード
ord-4cb0ea9eda0648f09d96a439cc915e21
出典データセット
uspto-grants-1998_06
特許番号
US05763552

関連ノート

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