反应 #314813

反应方程式

suspension

2-amino-4-(4-nitrophenyl)thiophene-3-carbonitrile

chloroformamidine hydrochloride

water

→

desired product

5-(4-nitrophenyl)thieno[2,3-d]pyrimidine-2,4-diamine

溶剂

diglyme

反应条件

后处理

1. 1
   萃取extracted twice with ethyl acetate
2. 2
   洗涤The combined extracts were washed with brine
3. 3
   干燥dried (MgSO4)
4. 4
   过滤filtered
5. 5
   浓缩concentrated
6. 6
   浓缩The residue was further concentrated under a stream of nitrogen
7. 7
   其他purified by silica gel chromatography with 5 to 7% methanol/dichloromethane

实验过程

A suspension of Example 58B (1 g, 4.08 mmol) and chloroformamidine hydrochloride (1.17 g, 10.2 mmol) in diglyme (40 mL) was heated to 130° C. for 15 hours. The mixture was cooled to room temperature, diluted with water, and extracted twice with ethyl acetate. The combined extracts were washed with brine, dried (MgSO4), filtered, and concentrated. The residue was further concentrated under a stream of nitrogen, and purified by silica gel chromatography with 5 to 7% methanol/dichloromethane to provide 0.26 g of the desired product. MS (ESI(+)) m/e 288 (M+H)+.

来源