HRID862577

反应详情

EQUATION

反应方程式

HRID 862577 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (S)-9-chloro-5-[p-tert-butoxycarbonylaminomethyl-o-(methoxycarbonylmethyl)phenylcarbamoylmethyl]-6,7-dihydro-1H, 5H -pyrido[1,2,3-de]quinoxaline-2,3-dione (1.82 g, 3.18 mmol) in a mixture of 1N aqueous sodium sulfate (20 mL), THF (20 mL), and methanol (20 mL) was stirred for 4 h at room temperature. The mixture was acidified to pH 3 by addition of 5% potassium hydrogen sulfate and extracted with a 1:1 mixture of ethyl acetate and THF. The organic layers were washed with brine, dried over magnesium sulfate, and concentrated. The residual solid was washed with dichloromethane, and dried in vacuo to give 1.499 g of the title compound.

WORKUP

后处理

  1. extractionextracted with a 1:1 mixture of ethyl acetate and THF
  2. washThe organic layers were washed with brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. washThe residual solid was washed with dichloromethane
  6. customdried in vacuo