Water → Diethyl 2-fluoro-2-phenylmalonate

HRID 1656807

반응식

HRID 1656807 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 4246642Diethyl 2-fluoro-2-phenylmalonate수율 47%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

반응 조건

온도
-20 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-89ade536182d46b086d4d518e6d9e093
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05254732

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