Dimethyl Sulfoxide → Ethyl 2-(3-fluoro-4-nitrophenyl)propanoate

HRID 2286467노트

반응식

HRID 2286467 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:11](C)([C:17](OCC)=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9].[Cl-].[Na+].CS(C)=O>O.C(OCC)(=O)C>[F:1][C:2]1[CH:3]=[C:4]([CH:11]([CH3:17])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:5]=[CH:6][C:7]=1[N+:8]([O-:10])=[O:9]

참가 물질

6

반응물 3

HCID 679Dimethyl SulfoxideHCID 5234Sodium ChlorideHCID 42638641,3-Diethyl 2-(3-fluoro-4-nitrophenyl)-2-methylpropanedioate

생성물 1

HCID 12879863Ethyl 2-(3-fluoro-4-nitrophenyl)propanoate

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 100 millimoles of diethyl 2-(3-fluoro-4-nitrophenyl)-2-methylmalonate, 110 millimoles of sodium chloride and 50 milliliters of dimethyl sulfoxide is heated under nitrogen at about 130° to 180° C. for about 6 hours. On cooling the mixture is diluted with 100 milliliters of water and 100 milliliters of ethyl acetate. The layers are separated and the organic layer is washed two times with 25 milliliters of water. After drying over disodium sulfate the organic layer is concentrated in vacuo to give the desired ethyl 2-(3-fluoro-4-nitrophenyl)propionate.

후처리

  1. temperatureis heated under nitrogen at about 130° to 180° C. for about 6 hours
  2. temperatureOn cooling the mixture
  3. customThe layers are separated
  4. washthe organic layer is washed two times with 25 milliliters of water
  5. dry with materialAfter drying over disodium sulfate the organic layer
  6. concentrationis concentrated in vacuo

출처 및 근거

ORD 기록
ord-54ff6a1ad6b44c1eb824ec42200e1064
출처 데이터셋
uspto-grants-1981_05
특허 번호
US04266069

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