Methanol → Methyl 2,2-difluoro-4-hydroxybutanoate

HRID 868405ノート

反応式

HRID 868405 の反応式
[F:1][C:2]([F:11])([CH2:7][C:8]([O-])=[O:9])[C:3]([O:5][CH3:6])=[O:4].CO>ClCCl.O1CCCC1>[F:1][C:2]([F:11])([CH2:7][CH2:8][OH:9])[C:3]([O:5][CH3:6])=[O:4]

参加物

5

反応物 2

HCID 887MethanolHCID 19860706HCID 19860706、化合物

生成物 1

HCID 13935576Methyl 2,2-difluoro-4-hydroxybutanoate

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

In a 4 L flask equipped with a reflux condenser and 1 L dropping funnel, a solution of BH3.Me2S complex (10M, 88 mL) in dry dichloromethane (1 L) is slowly added over a 2 hour period to a stirred solution of the methyl 2,2-difluorosuccinate (120 g, 0.714 moles) in dry tetrahydrofuran at 20° C. After refluxing (bath temperature 80° C.) for about 15 hours, the mixture is allowed to cool to room temperature and methanol (1 L) is slowly added. Evaporation yields methyl 2,2-difluoro-4-hydroxybutyrate as an oil which is stripped with methanol (1 L) and finally with CCl4 to yield a yellow oil: 100 g (92%).

後処理

  1. customIn a 4 L flask equipped with a reflux condenser
  2. temperatureto cool to room temperature
  3. customEvaporation

出典と根拠

ORDレコード
ord-25774f63ed54478ea46c22b3c3188ed8
出典データセット
uspto-grants-1988_10
特許番号
US04778926

反応ノート

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