HRID1927247
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
2-Amino-nicotinamide (1.6 g) described in Manufacturing Example 14-1, hexamethyldisiloxane (3.2 g), phosphorus pentasulfide (950 mg), and hexamethylphosphoramide (13 mL) were stirred for 18 hours at 110° C. The reaction solution was passed through a glass filter (eluted with ethyl acetate) lined with NH-silica gel and silica gel in a 1:1 ratio. The eluate was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1) to obtain the titled compound (290 mg).
WORKUP
后处理
- filtrationfilter
- wash(eluted with ethyl acetate)
- customThe eluate was purified by NH silica gel column chromatography (heptane:ethyl acetate=1:1)