Phosphorus tribromide → HCID 22494096、化合物

HRID 1816631ノート

反応式

HRID 1816631 の反応式
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]

参加物

5

反応物 2

HCID 24614Phosphorus tribromideHCID 22494341HCID 22494341、化合物

生成物 1

HCID 22494096HCID 22494096、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-503ae909041e4040a24f0d42193a730b
出典データセット
uspto-grants-2005_04
特許番号
US06884821B1

反応ノート

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