HRID1106654

反应详情

EQUATION

反应方程式

HRID 1106654 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The N-Boc p-hydroxy phenyl glycine methyl ester from step (300a) (123.0 g, 440 mmol) was combined with benzyl bromide (90.3 g, 528 mmol), potassium carbonate (182 g, 1.3 mol) and acetone (800 mL) under a nitrogen atmosphere. The reaction was heated to reflux for 5 h, allowed to cool to rt, diluted with ethyl acetate (800 mL) filtered to remove the solids and concentrated in vacuo to give a semisolid residue. The product was crystallized from ethyl ether to give the N-Boc p-benzyloxy phenyl glycine methyl ester (106.7 g, 65%) as a white powder. MS (M+H)+ =372, (M+NH4)+ =389.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 5 h
  3. filtrationfiltered
  4. customto remove the solids
  5. concentrationconcentrated in vacuo
  6. customto give a semisolid residue
  7. customThe product was crystallized from ethyl ether