HRID853889

反应详情

EQUATION

反应方程式

HRID 853889 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5′-Amino-1′-(3-aminopropyl)spiro[1,3-dioxane-2,3′-indol]-2′(1′H)-one (1.56 g, 5.63 mmol) was dissolved in 2M EtOAc.NH3 (1.90 mL) and THF (10 mL) and heated in a steel pressure vessel at 135° C. for 16 hr. The reaction mixture was cooled to room temperature and combined with silica gel and concentrated. The adsorbate was purified on Biotage KP silica gel eluting with a step gradient of CH2Cl2/CH3OH/NH4OH (95/3/2) to (85/10/5) to give the title compound as a bright yellow-orange solid (1.11 g, 76% yield). NMR (300 Mz, DMSO-d6): consistent.

WORKUP

后处理

  1. concentrationconcentrated
  2. customThe adsorbate was purified on Biotage KP silica gel eluting with a step gradient of CH2Cl2/CH3OH/NH4OH (95/3/2) to (85/10/5)