HRID453491

反应详情

EQUATION

反应方程式

HRID 453491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

The product of step A (2.5 g, 6.80 mmol) was diluted with 7N ammonia/methanol (30 mL) followed by the addition of Raney Nickel (0.0583 g, 0.680 mmol). The reaction mixture was purged three times with hydrogen and stirred for 12 hours. The reaction mixture was then filtered through a GF/F filter and concentrated. The residue was purified using a biotage 40M column eluting with methylene chloride:MeOH:NH4OH (90:9:1) to yield methyl 4-(2-(aminomethyl)-4-(2-tert-butoxy-2-oxoethyl)phenoxy)benzoate (1.87 g, 74.0% yield) as a clear oil.

WORKUP

后处理

  1. customThe reaction mixture was purged three times with hydrogen
  2. filtrationThe reaction mixture was then filtered through a GF/F
  3. filtrationfilter
  4. concentrationconcentrated
  5. customThe residue was purified
  6. washeluting with methylene chloride:MeOH:NH4OH (90:9:1)