反应详情

To a suspension of polymer supported Hünig's base (0.11 g, 0.40 mmol) and 52 (0.03 g, 0.066 mmol) in dry dichloromethane (1 ml) was added α-chloroethyl chloroformate (0.09 g, 0.066 mmol) at room temperature under nitrogen. The mixture was stirred at room temperature over the weekend then filtered and concentrated in vacuo. This was taken up in methanol, heated at 70° C. for 2 hours, cooled, and purified by SCX chromatography (eluent: ammonia/methanol 1/1 [v/v]) to give 9 as a colourless oil (0.01 g, 43%). The spectroscopic data for 9 obtained by the route outlined here was identical to the data for 9 obtained as described above.

1. additionTo a suspension of polymer
2. filtrationthen filtered
3. concentrationconcentrated in vacuo
4. temperatureheated at 70° C. for 2 hours
5. temperaturecooled
6. custompurified by SCX chromatography (eluent: ammonia/methanol 1/1 [v/v])