HRID1796242

反应详情

EQUATION

反应方程式

HRID 1796242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(2R,4R)-4-Hydroxy-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester (1.5 g, 6.5 mmol) was dissolved in 20 mL DMF, added imidazole (1.1 g, 16 mmol), dimethylaminopyridine (80 mg, 0.65 mmol), and tert-butyldimethylsilyl chloride (1.08 g, 7.1 mmol). Stirred at ambient temperature overnight, dissolved in 150 mL EtOAc, washed with 10% citric acid (3×100 mL), water (2×100 mL), brine, dried with MgSO4, filtered, and concentrated. Redissolved in 50 mL CHCl3 and reconcentrated to yield title compound as a clear oil. (1.54 g, 69%) APCI (AP−): 344.2 (M−H)−.

WORKUP

后处理

  1. washwashed with 10% citric acid (3×100 mL), water (2×100 mL), brine
  2. dry with materialdried with MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. dissolutionRedissolved in 50 mL CHCl3