HRID2100370

反应详情

EQUATION

反应方程式

HRID 2100370 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

LiOH (1N, 9 mL, 5 mmol) was added into a mixture of methyl 2-(4-(bis(benzyloxy)phosphoryloxy)phenyl)acetate (1.53 g, 3.59 mmol) in THF (15 mL) and methanol (5 mL) at 0° C. The reaction was stirred at 0° C. for 3.5 h, than 0.5 h at rt. The reaction was monitored by LC-MS until the hydrolysis was completed. The mixture was cooled to 0° C. and acidified by 1N HCl to pH=2. The mixture was concentrated and extracted by ethyl acetate (50 mL×3). The extraction was dried over Na2SO4 and concentrated to dryness to give the acid (1.5 g, 67.6% yield) as a light yellow oil.

WORKUP

后处理

  1. temperatureThe mixture was cooled to 0° C.
  2. concentrationThe mixture was concentrated
  3. extractionextracted by ethyl acetate (50 mL×3)
  4. extractionThe extraction
  5. dry with materialwas dried over Na2SO4
  6. concentrationconcentrated to dryness