反应详情

温度

10 °C

A solution of sulphur dichloride (11.3 g) in dichloromethane (10 ml) was added over 20 minutes to a solution of N-methylbutanamide (10.1 g) in the same solvent (35 ml) with stirring, the temperature being maintained at 10° C. Stirring at this temperature was continued for a further 30 minutes after which time a solution of pyridine (8.7 g) in dichloromethane (15 ml) was added. The mixture was then stirred and allowed to warm to room temperature over 2 hours, then filtered. The solvent was stripped off and the residue extracted with diethyl ether. After filtration, solvent removal and distillation, 12.1 g of the sulphenyl chloride as an oil, boiling point 82°-84° C. at 13 mmHg, was obtained. 4.4 g of this oil was dissolved in diethyl ether (10 ml) and the resulting solution was added over 20 minutes to a mixture of the compound of Example 1 (7.6 g) and triethylamine (2.7 g) in diethyl ether (30 ml). After stirring for 30 minutes at room temperature, 150 ml diethyl ether was added, the resultant soution was washed three times with water, dried, stripped of solvent and purified by chromatography over silica using dichloromethane as eluant. 9.1 g of the desired product was obtained as a brown oil.

1. stirringStirring at this temperature
2. stirringThe mixture was then stirred
3. temperatureto warm to room temperature over 2 hours
4. filtrationfiltered
5. extractionthe residue extracted with diethyl ether
6. filtrationAfter filtration, solvent removal and distillation, 12.1 g of the sulphenyl chloride as an oil, boiling point 82°-84° C. at 13 mmHg
7. customwas obtained
8. stirringAfter stirring for 30 minutes at room temperature
9. washthe resultant soution was washed three times with water
10. customdried
11. custompurified by chromatography over silica