反应详情

温度

60 °C

Concentrated HCl (2 ml) is added to a suspension of (S)-2-methyl-pyrrolidine-2-carboxylic acid (2 g) in butan-1-ol (50 ml) which is heated at 60° C. for 18 hours then at reflux for 4 days. The reaction mixture is evaporated, partitioned between saturated aqueous NaHCO3 and CH2Cl2, extracted 3×CH2Cl2, dried over Na2SO4 and evaporated. The isolated oil is then kugelrohr distilled at 10 mbar to give the title compound as a clear colorless oil from the fraction distilling at an oven temperature of 100-120° C.

1. temperatureat reflux for 4 days
2. customThe reaction mixture is evaporated
3. custompartitioned between saturated aqueous NaHCO3 and CH2Cl2
4. extractionextracted 3×CH2Cl2
5. dry with materialdried over Na2SO4
6. customevaporated
7. distillationThe isolated oil is then kugelrohr distilled at 10 mbar