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

HRID 747467

반응식

HRID 747467 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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-890678fea6054182989fef150ca76d42
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07396848B1

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