反应详情

温度

0 °C

A solution containing 3-hydroxy-pyrrolidine-1,2-dicarboxylic acid 1-tert-butyl ester (37, 16 g, 71 mmol)1 in DMF (100 mL) was cooled to 0° C. To this solution was added K2CO3 (16 g, 116 mmol) followed by iodomethane (5.4 mL, 87 mmol). The reaction mixture was slowly warmed to ambient temperature over 1 h at which time it became a yellow heterogeneous solution. This mixture was heated at 90° C. for 1 h and then cooled to ambient temperature. The solution was diluted with brine, extracted with diethyl ether, dried over anhydrous Na2SO4, filtered, and concentrated to afford 14.8 g (87%) of 38 as a yellow oil.2 1Hodges, J. A.; Raines, R. T. J. Am. Chem. Soc. 2005, 45, 15923.2Demange, I.; Cluzeau, J.; Menez, A.; Dugave, C. Tetrahedron Lett. 2001, 42, 651.

1. temperatureThe reaction mixture was slowly warmed to ambient temperature over 1 h at which time it
2. temperatureThis mixture was heated at 90° C. for 1 h
3. temperaturecooled to ambient temperature
4. extractionextracted with diethyl ether
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated