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

HRID 267388

반응식

HRID 267388 반응식
[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]

참가 물질

3

반응물 2

HCID 62678Phosphorus pentabromideHCID 21556089Ethyl 2'-chloro-4-biphenylylglycolate

생성물 1

HCID 21556258Ethyl alpha-bromo-2'-chloro-4-biphenylylacetate

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-972bcdda42be47e491f931bf35cb1fed
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941821

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