反应详情

温度

100 °C

Add sodium ethoxide (145 g, 2.03 mol), followed by toluene (7 L) and 3-(2-oxo-pyrrolidin-1-ylimino)-3-pyridin-2-yl-propionic acid ethyl ester (Preparation 3-B; 280 g, 1.02 mol) to a 22 L flask equipped with mechanical stirrer, nitrogen inlet and a reflux condenser. Heat the mixture to 100° C. for 21 h. Cool to room temperature, add water (6 L), and adjust to pH 5 with concentrated hydrochloric acid. Separate the organic layer and extract the aqueous layer with 10% isopropyl alcohol in chloroform (2×9 L). Combine the organic layers, dry (sodium sulfate), filter, and concentrate in vacuo to yield 218 g (93%) of the title compound as a yellow solid MS ES+ m/e 230 (M+1).

1. customequipped with mechanical stirrer, nitrogen inlet and a reflux condenser
2. temperatureCool to room temperature
3. customSeparate the organic layer
4. extractionextract the aqueous layer with 10% isopropyl alcohol in chloroform (2×9 L)
5. dry with materialCombine the organic layers, dry (sodium sulfate)
6. filtrationfilter
7. concentrationconcentrate in vacuo