Dimethyl Sulfate → Methyl 3-methoxy-2-(alpha,alpha,alpha-trifluoro-m-tolyl)-acrylate

HRID 1109602노트

반응식

HRID 1109602 반응식
[OH:1][CH:2]=[C:3]([C:8]1[CH:9]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:12][CH:13]=1)[C:4]([O:6][CH3:7])=[O:5].S(OC)(O[CH3:22])(=O)=O>[OH-].[Na+].O>[CH3:22][O:1][CH:2]=[C:3]([C:8]1[CH:9]=[C:10]([C:14]([F:15])([F:16])[F:17])[CH:11]=[CH:12][CH:13]=1)[C:4]([O:6][CH3:7])=[O:5]

참가 물질

5

반응물 2

HCID 6497Dimethyl Sulfate2회HCID 67828062Methyl 3-hydroxy-2-(alpha,alpha,alpha-trifluoro-m-tolyl)acrylate

생성물 1

HCID 53807060Methyl 3-methoxy-2-(alpha,alpha,alpha-trifluoro-m-tolyl)-acrylate

시약·촉매·용매 2

HCID 962Water용매HCID 14798Sodium Hydroxide용매2회

실험 절차

ba) 26 g of methyl 3-hydroxy-2-(α,α,α-trifluoro-m-tolyl)acrylate were dissolved in 1N sodium hydroxide solution while cooling in an ice-bath and treated with 10.6 ml of dimethyl sulfate. The mixture was stirred at about 0° for about 40 hours and an additional 40 ml of 1N sodium hydroxide solution and 3.8 ml of dimethyl sulfate were added. After the reaction was completed, the mixture was diluted with water and extracted with methylene chloride. After drying with sodium sulfate, the extract was distilled, whereby methyl 3-methoxy-2-(α,α,α-trifluoro-m-tolyl)-acrylate was obtained as a colorless oil of b.p. 75°-90°/0.2 mm.

후처리

  1. temperaturewhile cooling in an ice-bath
  2. extractionextracted with methylene chloride
  3. dry with materialAfter drying with sodium sulfate
  4. distillationthe extract was distilled

출처 및 근거

ORD 기록
ord-e3ca86c6b5984c1ca3f807b0eb24ee23
출처 데이터셋
uspto-grants-1994_06
특허 번호
US05321021

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