HRID1788353

反应详情

EQUATION

反应方程式

HRID 1788353 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of the product of Example 44A (2.16 g, 9.51 mmol) in CHCl3 (8 mL) was added, with ice cooling, pyrrolidine (4.05 g, 57.04 mmol). The mixture was stirred at 25° C. for 2 hrs, then concentrated in vacuo. The residue was dissolved in toluene, washed with HCl and water, dried (Na2SO4) and concentrated. The resulting oil was crystallized from hexane and chromatographed (CH2Cl2) to yield the title compound (1.92 g), m.p. 101-102° C.

WORKUP

后处理

  1. concentrationconcentrated in vacuo
  2. dissolutionThe residue was dissolved in toluene
  3. washwashed with HCl and water
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated
  6. customThe resulting oil was crystallized from hexane
  7. customchromatographed (CH2Cl2)