反应 #833554

反应方程式

triethylamin

3,4,6,7,8,9-hexahydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine 1,1-dioxide

p-fluor-phenylisocyanate

→

3,4,6,7,8,9-hexahydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine

收率 97.1%

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 2.3 g crude product
7. 7
   其他This material was recrystallized from ethanol

实验过程

0.76 g (7.5 mmol) triethylamin were added to a solution of 2 g (7.5 mmol) 3,4,6,7,8,9-hexahydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine 1,1-dioxide and 1.03 g (7.5 mmol) p-fluor-phenylisocyanate dissolved in 50 mL DMSO (dimethyl sulfoxide) at room temperature. After stirring for 1 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 2.3 g crude product. This material was recrystallized from ethanol to give 1.7 g 3,4,6,7,8,9-hexahydro-2-methyl-3-oxo-2H-naphtho[2,3-e]-1,2-thiazine-4-(4-fluor)carboxanilide 1,1-dioxide.

来源