Phosphorus pentabromide → Ethyl alpha-bromo-2'-chloro-4-biphenylylacetate

HRID 267388

反応式

HRID 267388 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH:14](O)[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:10][CH:9]=1.P(Br)(Br)(Br)(Br)[Br:22]>>[Br:22][CH:14]([C:11]1[CH:12]=[CH:13][C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[Cl:1])=[CH:9][CH:10]=1)[C:15]([O:17][CH2:18][CH3:19])=[O:16]

参加物

3

実験手順

To 15.0 g. (0.0476 moles) of ethyl 2'-chloro-4-biphenylylglycolate there is added slowly with stirring at 40°-50°C 23 g. (0.053 moles) of phosphorus pentabromide. The mixture is stirred at room temperature for 16 hours, then diluted with 70 ml. of petroleum ether, and poured into 125 ml. of ice-cold water. The organic phase is separated, washed with saturated aqueous sodium hydrogen carbonate solution, dried over anhydrous sodium sulfate, filtered and the solvent removed in vacuo to obtain ethyl α-bromo-2'-chloro-4-biphenylylacetate.

後処理

  1. stirringThe mixture is stirred at room temperature for 16 hours
  2. additiondiluted with 70 ml
  3. customThe organic phase is separated
  4. washwashed with saturated aqueous sodium hydrogen carbonate solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-972bcdda42be47e491f931bf35cb1fed
出典データセット
uspto-grants-1976_03
特許番号
US03941821

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