反应详情

温度

80 °C

Lawesson's reagent (0.69 g, 1.64 mmol, 1.3 eq.) was added in one portion to a suspension of 5-(3-amino-phenyl)-5-methyl-morpholin-3-one (0.26 g, 1.26 mmol) in 1,2-dimethoxyethane (10 ml); the reaction mixture was stirred at 80° C. for 18 hours. After complete conversion, the solvent was partially removed at reduced pressure and the dark orange oil diluted with dichloromethane (5 ml) before washing with 1 M HCl (2×5 ml). The aqueous phase was brought to pH 8 and extracted with dichloromethane (4×10 ml) to yield the (RS)-5-(3-amino-phenyl)-5-methyl-morpholine-3-thione as a yellow oil (0.16 g, 57% of theory). Mass (calculated) C11H14N2OS [222.31]; (found) [M+H]+=223.

1. customAfter complete conversion, the solvent was partially removed at reduced pressure
2. additionthe dark orange oil diluted with dichloromethane (5 ml)
3. washbefore washing with 1 M HCl (2×5 ml)
4. extractionextracted with dichloromethane (4×10 ml)