Phosphorus tribromide → 1-(1-Bromoethyl)-3-methylbenzene

HRID 2206542

反応式

HRID 2206542 の反応式
P(Br)(Br)[Br:2].[C:5]1([CH3:14])[CH:10]=[CH:9][CH:8]=[C:7]([CH:11](O)[CH3:12])[CH:6]=1>>[Br:2][CH:11]([C:7]1[CH:8]=[CH:9][CH:10]=[C:5]([CH3:14])[CH:6]=1)[CH3:12]

参加物

3

反応物 2

HCID 24614Phosphorus tribromideHCID 1109521-(3-Methylphenyl)ethanol

生成物 1

HCID 230009161-(1-Bromoethyl)-3-methylbenzene収率 91.3%

実験手順

Phosphorus tribromide (4.28 g, 15.9 mmol) was added drop-wise to a stirred neat solution of 1-(m-tolyl)ethanol (0.9 g, 6.6 mmol) at 0° C. After being stirred to room temperature over 12 h, the reaction was carefully quenched with sat'd saturated aqueous NaHCO3 solution and the mixture was extracted with EtOAc. The organic extract was washed with water, dried with MgSO4, and conc. in vacuo to afford the title compound (1.2 g, 91%) as a colorless oil, that was used directly in the next step without further purification. LCMS 200 (M+H+).

後処理

  1. customthe reaction was carefully quenched with sat'd saturated aqueous NaHCO3 solution
  2. extractionthe mixture was extracted with EtOAc
  3. extractionThe organic extract
  4. washwas washed with water
  5. dry with materialdried with MgSO4

出典と根拠

ORDレコード
ord-c35aa29ec8ad4d20905cedd6519d2cca
出典データセット
uspto-grants-2016_06
特許番号
US09371331B2

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