反应详情

A solution of methyl-2-azido-3-(4-methylthiophenyl)-propenoate (20.6 g, 83 mmol) in xylene (200 ml) was added dropwise to boiling xylene (250 ml) over a period of 2 hours. The reaction mixture was allowed to heat at reflux temperature for an additional 2 hours, then cooled slowly and placed in a freezer overnight. The solids were filtered, washed with a small amount of CH2Cl2 /hexane (1:3) and dried to give 11.2 g (61.0%) of methyl-6-methylsulfanyl-1H-indole-2-carboxylate.

1. customof 2 hours
2. temperatureto heat
3. temperatureat reflux temperature for an additional 2 hours
4. temperaturecooled slowly
5. filtrationThe solids were filtered
6. washwashed with a small amount of CH2Cl2 /hexane (1:3)
7. customdried