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

HRID 47936

반응식

HRID 47936 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-3bf23ac72d0e454e87c0e21c7a1e4332
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06699995B1

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