2-Bromo-1-(3,4-dichlorophenyl)ethanone → 1-(3,4-Dichlorophenyl)-2-hydroxyethan-1-one

HRID 47936

反応式

HRID 47936 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[C:7]([Cl:12])[CH:6]=1)=[O:4].C([O-])=[O:14].[Na+]>CO>[OH:14][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[C:7]([Cl:12])[CH:6]=1)=[O:4]

参加物

4

反応物 2

HCID 2447512-Bromo-1-(3,4-dichlorophenyl)ethanoneHCID 2723810Sodium Formate

生成物 1

HCID 70621931-(3,4-Dichlorophenyl)-2-hydroxyethan-1-one収率 42%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A mixture of 2-bromo-3′,4′-dichloroacetophenone (78.0 g), sodium formate (68.0 g) and methanol (300 mL) was heated under reflux and stirred for 16 h. The reaction mixture was concentrated and poured into water (1 L). The precipitated solid was collected by filtration, washed with water and then with isopropyl ether, air-dried, and further dried under reduced pressure at 40° C. to give the title compound as crystals (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale-yellow prism crystals. melting point: 115-118° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux
  3. concentrationThe reaction mixture was concentrated
  4. additionpoured into water (1 L)
  5. filtrationThe precipitated solid was collected by filtration
  6. washwashed with water
  7. dry with materialwith isopropyl ether, air-dried
  8. customfurther dried under reduced pressure at 40° C.

出典と根拠

ORDレコード
ord-3bf23ac72d0e454e87c0e21c7a1e4332
出典データセット
uspto-grants-2004_03
特許番号
US06699995B1

関連ノート

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