HRID1504847

反应详情

EQUATION

反应方程式

HRID 1504847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of benzyl tert-butyl (3-aminopropane-1,2-diyl)biscarbamate (8.0 g, 25 mmol) and triethylamine (7.9 g, 78 mmol) in DCM (100 mL) was added acetic anhydride (2.8 g, 27 mmol) at 0° C. After 1 hour, the reaction mixture was diluted with ethyl acetate. The organic layer was concentrated under reduced pressure and the residue was purified by chromatography on silica gel to give benzyl tert-butyl [3-(acetylamino)propane-1,2-diyl]biscarbamate. MS ESI calc'd. for C18H28N3O5 [M+H]+ 366. found 366. 1H NMR (400 MHz, CD3OD) δ 7.34-7.30 (m, 5H), 5.01 (s, 2H), 3.59-3.51 (m, 3H), 2.87-2.77 (m, 2H), 2.0 (s, 3H), 1.42 (s, 9H).

WORKUP

后处理

  1. concentrationThe organic layer was concentrated under reduced pressure
  2. customthe residue was purified by chromatography on silica gel