HRID1501969

反应详情

EQUATION

反应方程式

HRID 1501969 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 3-(2-methoxy-2-oxoethyl)piperazine-1-carboxylate (7.28 g, 28.2 mmol) was dissolved in THF (100 mL) at 0° C. then added LAH (21.14 mL, 21.14 mmol). The reaction was monitored by TLC. After 30 mins, the reaction was first quenched with 0.8 mL water, then added 1.6 mL 2N NaOH followed by 4 mL water. The above slurry was diluted with ethyl acetate and MgSO4 was added. The mixture was stirred at RT for ½ h, then filtered and concentrated to yield the title compound: LC-MS (IE, m/z): 231 [M+1]+.

WORKUP

后处理

  1. customthe reaction was first quenched with 0.8 mL water
  2. additionadded 1.6 mL 2N NaOH
  3. additionThe above slurry was diluted with ethyl acetate and MgSO4
  4. additionwas added
  5. filtrationfiltered
  6. concentrationconcentrated