反应详情

Sulfuric acid (conc., 1.704 g, 0.926 mL, 17.37 mmol) was added to a solution of (S)-2-amino-2-cyclopropylacetic acid (1 g, 8.69 mmol) in ethanol (12 mL) and heated to reflux for 5 h, then cooled to rt. The reaction mixture was concentrated under vacuum to remove solvent and water (10 mL) was added. The pH of the mixture was adjusted to 10 using 2M aq. sodium hydroxide and was then extracted with DCM (3×15 mL). The organic phase was dried with sodium sulfate and concentrated under vacuum to provide (S)-ethyl 2-amino-2-cyclopropylacetate (862 mg) which was used as is.

1. temperatureheated
2. temperatureto reflux for 5 h
3. concentrationThe reaction mixture was concentrated under vacuum
4. customto remove solvent and water (10 mL)
5. additionwas added
6. extractionwas then extracted with DCM (3×15 mL)
7. dry with materialThe organic phase was dried with sodium sulfate
8. concentrationconcentrated under vacuum