HRID635155

反应详情

EQUATION

反应方程式

HRID 635155 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Methyl-3-phenylpropanol (219 g., 1.46 mol.) and 10.30 g. of 50% Ni on silica catalyst (4.7 wt %, G-49-C, United Catalyst) were stirred at 700 rpm in a Parr reactor at 150° C. and 200-600 psi of hydrogen until hydrogen absorption stopped (12 hours). Utilizing 2 wt. % of the catalyst requires that the reaction be run at 180° C. The reaction mixture was filtered through a filter bed (Celite™) using toluene as a rinse solvent and concentrated to a clear, colorless liquid. The odor grade product was isolated by fractional distillation, 174 g., 80% yield; bp 80° C. at 4 mm. Odor: very pleasant green, fruity, rosy. Mass Spectrum from 5508-36. MS (El) m/z (relative intensity) 138 (M+−H2O, 15), 123 (M+−Me and H2O, 15).

WORKUP

后处理

  1. custom200-600 psi of hydrogen until hydrogen absorption
  2. custom(12 hours)
  3. custombe run at 180° C
  4. filtrationThe reaction mixture was filtered through a filter bed (Celite™)
  5. concentrationconcentrated to a clear, colorless liquid
  6. customThe odor grade product was isolated by fractional distillation, 174 g