反应 #312637

反应方程式

3-[(4-chloro-2,5-difluorobenzoyl)amino]thiophene-2-carboxylic acid

thionyl chloride

DMF

→

2-(4-chloro-2,5-difluorophenyl)thieno[3,2-d]pyrimidine-4(1H)-one

反应条件

后处理

1. 1
   其他the solvent was removed under reduced pressure and 1,4-dioxane
2. 2
   workup.ADDITIONwas added
3. 3
   workup.ADDITIONAfter the reaction solution was added to 28% ammonia water under ice cooling
4. 4
   workup.STIRRINGstirred at room temperature for 3 hours
5. 5
   其他the solvent was removed under reduced pressure
6. 6
   workup.ADDITIONMeOH and 1M NaOH aq were added to the obtained residue
7. 7
   workup.STIRRINGstirred for 2.5 hours at 90° C.

实验过程

After a mixture of 3-[(4-chloro-2,5-difluorobenzoyl)amino]thiophene-2-carboxylic acid, thionyl chloride and DMF was stirred for 1.5 hours at 75° C., the solvent was removed under reduced pressure and 1,4-dioxane was added. After the reaction solution was added to 28% ammonia water under ice cooling and stirred at room temperature for 3 hours, the solvent was removed under reduced pressure. MeOH and 1M NaOH aq were added to the obtained residue and stirred for 2.5 hours at 90° C. to give 2-(4-chloro-2,5-difluorophenyl)thieno[3,2-d]pyrimidine-4(1H)-one.

来源