Phosphorus tribromide → HCID 14149585、化合物

HRID 1733281ノート

反応式

HRID 1733281 の反応式
[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]

参加物

3

反応物 2

HCID 24614Phosphorus tribromideHCID 92013Benzenepropanol, 4-(1,1-dimethylethyl)-beta-methyl-

生成物 1

HCID 14149585HCID 14149585、化合物

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3269b6a14cf7436eb2ddceef8a2aaccc
出典データセット
uspto-grants-1980_12
特許番号
US04241058

反応ノート

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