Water → Ethyl cyclohexylideneacetate

HRID 1769582ノート

反応式

HRID 1769582 の反応式
[CH3:1][C:2](C)([O-:4])C.[K+].FC1C=[C:10]([CH:16]2[CH2:21][CH2:20][C:19](=O)[CH2:18][CH2:17]2)[CH:11]=C(F)C=1F.[OH2:23]>C1COCC1>[CH2:2]([O:4][C:11]([CH:10]=[C:16]1[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21]1)=[O:23])[CH3:1]

参加物

5

反応物 3

HCID 962WaterHCID 219932844-(3,4,5-Trifluorophenyl)cyclohexan-1-oneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 73776Ethyl cyclohexylideneacetate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A suspension of triethyl phosphonoacetate (21.8 g) in THF (50 ml) was stirred in a nitrogen gas stream, followed by adding potassium-t-butoxide (11.8 g) little by little at room temperature, stirring the reaction solution at room temperature for one hour, dropwise adding a solution of 4-(3',4',5'-trifluorophenyl)cyclohexanone (20 g) in THF (50 ml), stirring at room temperature for 2 hours, adding to water (100 ml), extracting with ethyl acetate (100 ml), washing the organic layer with water, drying over anhydrous MgSO4 and concentrating the solvent under reduced pressure, to obtain 4-(3',4',5'-trifluorophenyl))ethoxycarbonylmethylenecyclohexane (18.3 g).

後処理

  1. stirringstirring the reaction solution at room temperature for one hour
  2. stirringstirring at room temperature for 2 hours
  3. extractionextracting with ethyl acetate (100 ml)
  4. washwashing the organic layer with water
  5. dry with materialdrying over anhydrous MgSO4
  6. concentrationconcentrating the solvent under reduced pressure

出典と根拠

ORDレコード
ord-06f97a4fe8a04746bd885910931cd362
出典データセット
uspto-grants-1995_01
特許番号
US05382379

反応ノート

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