反应详情

To a solution of 383.4 mg of 14 and 4.0 mL toluene in a 10 mL round-bottom flask equipped with a magnetic stirrer, a reflux condenser maintained under an argon atmosphere at RT was added, 191 μl of triethyl phosphite. Nitrogen evolution began in about 5 min and after 30 min at RT the light yellow reaction mixture was heated to reflux for 5 h, then an additional 191 μl of triethyl phosphite were added and refluxing continued for another 2 h. The reaction mixture was cooled and evaporated at 40° C./60-10 mbar to yield 470 mg of the crude product as a yellow oil. The crude product was purified by SiO2 column chromatography using a 2/1 mixture of toluene and acetone. The combined fractions were evaporated and dried on a rotary evaporator 40° C./250-10 mbar to afford 87 mg of 16 as a yellow oil.

1. additionwas added
2. temperaturethe light yellow reaction mixture was heated
3. temperatureto reflux for 5 h
4. temperaturerefluxing
5. waitcontinued for another 2 h
6. temperatureThe reaction mixture was cooled
7. customevaporated at 40° C./60-10 mbar
8. customto yield 470 mg of the crude product as a yellow oil
9. customThe crude product was purified by SiO2 column chromatography
10. additiona 2/1 mixture of toluene and acetone
11. customThe combined fractions were evaporated
12. customdried on a rotary evaporator 40° C./250-10 mbar