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

HRID 477955ノート

反応式

HRID 477955 の反応式
[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]

参加物

5

反応物 2

HCID 6497Dimethyl Sulfate2 回HCID 67828062Methyl 3-hydroxy-2-(alpha,alpha,alpha-trifluoro-m-tolyl)acrylate

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒2 回

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-8c92c3eabb454bcca6328ad9f06a4c84
出典データセット
uspto-grants-1989_12
特許番号
US04889848

反応ノート

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