Water → Diethyl 2-fluoro-2-phenylmalonate

HRID 1656807

反応式

HRID 1656807 の反応式
[C:1]1([CH:7]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[H-].[K+].C1C=CC(S(N(S(C2C=CC=CC=2)(=O)=O)[F:30])(=O)=O)=CC=1.O>CCOCC>[C:1]1([C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])([C:13]([O:15][CH2:16][CH3:17])=[O:14])[F:30])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

6

反応物 4

HCID 962WaterHCID 66514Diethyl phenylmalonateHCID 82127Potassium hydrideHCID 588007N-Fluorobenzenesulfonimide

生成物 1

HCID 4246642Diethyl 2-fluoro-2-phenylmalonate収率 47%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
-20 °C

実験手順

1 millimole of diethyl phenylmalonate was stirred with potassium hydride in 2 milliliters ether for 30 minutes at -25° C. 1.2 molar equivalents N-fluorobenzenesulfonimide prepared according to Example 1 above in 2 milliliters ether were dropped into the mixture which was stirred for 1 hour at -20° C. The mixture was allowed to warm up to room temperature and water was added. The product was extracted into ether which was dried and evaporated. Purification was carried out on a silica gel column. C6H5CF(COOCH2CH3)2 was obtained in 47% yield.

後処理

  1. additionwere dropped into the mixture which
  2. temperatureto warm up to room temperature
  3. extractionThe product was extracted into ether which
  4. customwas dried
  5. customevaporated
  6. customPurification

出典と根拠

ORDレコード
ord-89ade536182d46b086d4d518e6d9e093
出典データセット
uspto-grants-1993_10
特許番号
US05254732

関連ノート

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