反应 #833556

反应方程式

3,4-dihydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine 1,1-dioxide

triethylamin

phenylisocyanate

→

3,4-dihydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine-4-carboxanilide 1,1-dioxide

收率 37.0%

溶剂

DMSO

反应条件

后处理

1. 1
   其他was quenched with dilute HCl in an ice bath
2. 2
   萃取extracted with ether (2 times)
3. 3
   洗涤The combined ether extracts were washed
4. 4
   其他dried
5. 5
   浓缩concentrated
6. 6
   其他to give 1.9 g crude product
7. 7
   其他This material was recrystallized from ethanol
8. 8
   其他followed by recrystallization from ethylacetate

实验过程

To a solution of 1.3 g (5 mmol) 3,4-dihydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine 1,1-dioxide and 0.7 ml (5 mmol) triethylamin dissolved in 10 ml DMSO at room temperature was added 0.6 g (5 mmol) phenylisocyanate. After stirring for 20 hr the resulting mixture was quenched with dilute HCl in an ice bath and then extracted with ether (2 times). The combined ether extracts were washed, dried and concentrated to give 1.9 g crude product. This material was recrystallized from ethanol followed by recrystallization from ethylacetate to give 0.7 g 3,4-dihydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine-4-carboxanilide 1,1-dioxide.

来源