HRID587801

反应详情

EQUATION

反应方程式

HRID 587801 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Chlorocyclooctadiene rhodium(I) dimer (0.217 g, 0.881 mmol of Rh), Josiphos SL-J216-2 (0.595 g, 0.926 mmol), and N-(1-benzyl-7-bromo-3,4-dihydronaphthalen-2-yl)propionamide (10.88 g, 29.4 mmol) were combined in a metal reactor, and the vessel was inerted with argon. Degassed ethanol (163 ml) was added, and the mixture was agitated under argon for 30 min at 50° C. The vessel was pressurized with 60 psig of hydrogen and agitated at 55° C. for 14.5 hrs. HPLC analysis indicated 89.4% conversion and 93.8% ee. The mixture was concentrated, and the resulting solid was crystallized from MeOH to yield 7.41 g (yield: 68%) of the title compound.

WORKUP

后处理

  1. stirringagitated at 55° C. for 14.5 hrs
  2. concentrationThe mixture was concentrated
  3. customthe resulting solid was crystallized from MeOH