反应 #171891

反应方程式

Pyridine

8-fluoro-4H-thieno[3,2-c]chromene-2-carbonyl chloride

2,4-difluoroaniline

→

N-(2,4-difluorophenyl)-8-fluoro-N-methyl-4H-thieno[3,2-c]chromene-2-carboxamide

收率 31.0%

溶剂

methylene chloride

反应条件

后处理

1. 1
   其他To a reaction
2. 2
   浓缩After aqueous work up, the reaction was concentrated in vacuo
3. 3
   浓缩a concentrated of 100 mg/ml
4. 4
   其他purified by preparative RP-HPLC
5. 5
   其他to give 163bp

实验过程

To a reaction vial charged with 8-fluoro-4H-thieno[3,2-c]chromene-2-carbonyl chloride (0.120 g, 0.447 mmol) and 2,4-difluoroaniline (0.0959 g, 0.670 mmol) was added a catalytic amount of DMAP. Pyridine in methylene chloride (1.2 M, 1.49 mL) was added. The reaction was stirred at room temperature with LC/MS monitor. The reaction was complete in a couple hours. After aqueous work up, the reaction was concentrated in vacuo, taken into DMF at a concentrated of 100 mg/ml and purified by preparative RP-HPLC to give 163bp. Yield=31% of theoretical. MS: (ESI+)=376.4

来源