Phosphorus tribromide → HCID 14149585, 화합물

HRID 1733281

반응식

HRID 1733281 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH:12]([CH3:15])[CH2:13]O)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].P(Br)(Br)[Br:17]>>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH:12]([CH3:15])[CH2:13][Br:17])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

3

실험 절차

300.2 g of 3-(p-tert.butyl-phenyl)-2-methyl-propanol are added dropwise over a period of 2 hours at 20°-30° C. to 218.6 g of phosphorus tribromide and the mixture is left to stand for 16 hours. The mixture is subsequently heated to 55°-60° C. over a period of 1.5 hours, cooled to ca 10° C. and cautiously poured on to ice. The aqueous solution is exhaustively extracted with ether, the combined ether phases are washed with saturated sodium bicarbonate solution and water, dried over sodium sulphate and evaporated. By fraction distillation there is obtained pure 3-(p-tert.butyl-phenyl)-2-methyl-propyl bromide of boiling point 104° C./0.025 Torr.

후처리

  1. waitthe mixture is left
  2. temperatureThe mixture is subsequently heated to 55°-60° C. over a period of 1.5 hours
  3. temperaturecooled to ca 10° C.
  4. additioncautiously poured on to ice
  5. extractionThe aqueous solution is exhaustively extracted with ether
  6. washthe combined ether phases are washed with saturated sodium bicarbonate solution and water
  7. dry with materialdried over sodium sulphate
  8. customevaporated
  9. distillationBy fraction distillation

출처 및 근거

ORD 기록
ord-3269b6a14cf7436eb2ddceef8a2aaccc
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04241058

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