反应详情

Dissolve 6-Methanesulfonyl-indol-1-ol (5.0 g, 23.7 mmol) in triethyl phosphite (35 ml) and heat at 160° for 5 hours. Cool the solution to ambient temperature and dilute with diethyl ether. Wash the ether solution with brine and water followed by drying (sodium sulfate) and reducing to residue. Crystallize the residue from warm ethyl acetate to give the title compound as colorless cubes: mp 149-152° C. MS (ACPI): m/e 196.0 (M+1). Analysis for C9H9NO2S: Calcd: C, 55.37; H, 4.65; N, 7.17. found: C, 55.14; H, 4.71; N, 7.20.

1. temperatureheat at 160° for 5 hours
2. washWash the ether solution with brine and water
3. dry with materialby drying (sodium sulfate)
4. customCrystallize the residue
5. temperaturefrom warm ethyl acetate