HRID727524

反应详情

EQUATION

反应方程式

HRID 727524 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

TFA (10.0 mL) is added to a solution of tert-butyl α-methyl-3-(2-methylpropyl)-2-oxo-1-(2-phenylethyl)-3-pyrrolidineacetate (780 mg, 2.09 mmol) and CH2Cl2 (10 mL) at 0° C. The solution is stirred for 2.5 hours at 0° C. and 1.5 hours at room temperature. After concentration, the residue is partitioned between EtOAc and water. The organic layer is extracted several times with 10% NaOH, the combined basic layers acidified (4N HCl), and the acidic layers extracted several times with CH2Cl2. The CH2Cl2 layers are dried (MgSO4), filtered, and concentrated to provide 79 mg (12%) of the title compound as a white solid (mp 94°-95° C.).

WORKUP

后处理

  1. concentrationAfter concentration
  2. customthe residue is partitioned between EtOAc and water
  3. extractionThe organic layer is extracted several times with 10% NaOH
  4. extractionthe acidic layers extracted several times with CH2Cl2
  5. dry with materialThe CH2Cl2 layers are dried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated