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

HRID 563114

反応式

HRID 563114 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 stirred with heating under reflux for 16 hours. The reaction mixture was concentrated and poured into water (1 L). The solid precipitates were filtered, washed with water and then isopropyl ether, and air-dried. The residue was dried under reduced pressure to give crystals of 2-hydroxy-3′,4′-dichloroacetophenone (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale yellow prisms. Melting point 115-118° C.

後処理

  1. temperaturewith heating
  2. temperatureunder reflux for 16 hours
  3. concentrationThe reaction mixture was concentrated
  4. additionpoured into water (1 L)
  5. customThe solid precipitates
  6. filtrationwere filtered
  7. washwashed with water
  8. dry with materialisopropyl ether, and air-dried
  9. customThe residue was dried under reduced pressure

出典と根拠

ORDレコード
ord-bb8838da0a3241e48202e46f87070be9
出典データセット
uspto-grants-2011_11
特許番号
US08067453B2

関連ノート

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