反应详情

温度

90 °C

A solution of 3.3 (110 mg, 0.318 mmol) and AIBN (21 mg, 0.127 mmol) in dry toluene (10 ml) was degassed for 15 mins with N2 and then heated to 90° C. Bu3SnH (84 μl, 0.318 mmol) was added to the mixture in four portions over an hour and the resulting mixture was stirred at 90° C. for a further 2 h. The mixture was then concentrated and purified by flash chromatography (SiO2, 0–10% EtOAc in hexane) to afford 3.4 (50 mg, 59%) as a colourless oil.FAB MS: (NBA/NaI) 267, (M+H+, expected 267) 292 (M+Na+, expected 292).

1. concentrationThe mixture was then concentrated
2. custompurified by flash chromatography (SiO2, 0–10% EtOAc in hexane)