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Phosphorus tribromide → HCID 19981886, 화합물

HRID 1460457
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HRID 1460457 반응식
O[CH:2]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([O:16][CH3:17])[CH:9]=1)[C:3]([O:5][CH2:6][CH3:7])=[O:4].P(Br)(Br)[Br:19]>C1C=CC=CC=1>[Br:19][CH:2]([C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([O:16][CH3:17])[CH:9]=1)[C:3]([O:5][CH2:6][CH3:7])=[O:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24614Phosphorus tribromideHCID 122605Benzeneacetic acid, .alpha.-hydroxy-3,4-dimethoxy-, ethyl ester

생성물 1

HCID 19981886HCID 19981886, 화합물수율 75%

시약·촉매·용매 1

HCID 241Benzene용매

반응 조건

온도
60 °C

실험 절차

To a solution of ethyl 2-hydroxy-2-(3,4-dimethoxyphenyl)acetate (19.5 g) in benzene (200 ml) was added phosphorus tribromide (8.18) dropwise at 50° C. and the mixture was stirred at 60° C. for one hour. The reaction mixture was then washed successively with water, saturated aqueous solution of NaHCO3 and water and dried (MgSO4). The benzene was distilled off and the residue was subjected to silica gel chromatography. From the fraction eluted by ethyl acetate-hexane (1:3, v/v), ethyl 2-bromo-2-(3,4-dimethoxyphenyl)acetate (18.5 g, yield 75%) was obtained as an oil.

후처리

  1. washThe reaction mixture was then washed successively with water, saturated aqueous solution of NaHCO3 and water
  2. dry with materialdried (MgSO4)
  3. distillationThe benzene was distilled off
  4. washFrom the fraction eluted by ethyl acetate-hexane (1:3

출처 및 근거

ORD 기록
ord-cd0d5babd3c54a6fb5fdc3ea610d0e88
출처 데이터셋
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05071841

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