Phosphorus tribromide → HCID 22494096, 화합물

HRID 1816631노트

반응식

HRID 1816631 반응식
O[CH2:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([O:18][CH:19]([CH3:21])[CH3:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].P(Br)(Br)[Br:23]>C(COC)OC.CCOCC>[Br:23][CH2:2][C:3]1[CH:4]=[C:5]([CH2:11][CH:12]([O:18][CH:19]([CH3:21])[CH3:20])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

참가 물질

5

반응물 2

HCID 24614Phosphorus tribromideHCID 22494341HCID 22494341, 화합물

생성물 1

HCID 22494096HCID 22494096, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 80711,2-Dimethoxyethane용매

실험 절차

2.2 g of ethyl 3-[3-(hydroxymethyl)-4-methoxyphenyl]-2-isopropoxypropanoate was dissolved in 15 ml dimethoxyethane. 1.2 ml phosphorus tribromide was added thereto under ice-cooling, followed by stirring at room temperature for 4 hours. The reaction solution was diluted with ether and washed with water. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and the solvent was evapoarated. The residue was subjected to silica gel column chromatography, to give 2.6 g of ethyl 3-[3-(bromomethyl)-4-methoxyphenyl]-2-isopropoxypropanoate from fractions eluted with hexane-ethyl acetate (4:1).

후처리

  1. temperatureunder ice-cooling
  2. washwashed with water
  3. washThe organic layer was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-503ae909041e4040a24f0d42193a730b
출처 데이터셋
uspto-grants-2005_04
특허 번호
US06884821B1

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