HRID454438

反应详情

EQUATION

反应方程式

HRID 454438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2-(1,1-dimethylethyl) 7-ethyl 2,6-diazaspiro[3.4]octane-2,7-dicarboxylate (145) (500 mg, 1.76 mmol), HATU (735 mg, 1.93 mmol) and N-[(methyloxy)carbonyl]-L-valine (339 mg, 1.93 mmol) in anhydrous CH2Cl2 (10 mL) was added Hunig's base (0.68 mL, 3.87 mmol) and the reaction stirred at room temperature under nitrogen for 2 h. The reaction was concentrated in vacuo and purified by C18 reverse-phase chromatography eluting with 10-90% ACN/water/0.2% NH4OH to afford the title compound as an off-white solid (398 mg, 51% yield).

WORKUP

后处理

  1. concentrationThe reaction was concentrated in vacuo
  2. custompurified by C18 reverse-phase chromatography
  3. washeluting with 10-90% ACN/water/0.2% NH4OH