반응 #833556

반응 방정식

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

수율 37.0%

용매

DMSO

반응 조건

후처리

1. 1
   기타was quenched with dilute HCl in an ice bath
2. 2
   추출extracted with ether (2 times)
3. 3
   세척The combined ether extracts were washed
4. 4
   기타dried
5. 5
   농축concentrated
6. 6
   기타to give 1.9 g crude product
7. 7
   기타This material was recrystallized from ethanol
8. 8
   기타followed by recrystallization from ethylacetate

실험 절차

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.

출처