反应详情

Nitrile 23-3 (400 mg, 2.11 mmol) was dissolved in 10 mL Et2O at 0° MeOH (289 μL, 4.2 mmol) was added, the mixture was saturated with anhydrous HCl. Once the white ppt. formed, the solvent was evaporated and replaced with MeOH (5 mL), cooled to 0°, and aminoacetaldehyde dimethylacetal (250 μL, 2.3 mmol) was added. The reaction was heated to reflux for 3 days then concentrated, diluted in 10 mL 6 N HCl and concentrated again providing 23-4 as a solid.

1. additionwas added
2. customformed
3. customthe solvent was evaporated
4. temperaturecooled to 0°
5. temperatureThe reaction was heated
6. temperatureto reflux for 3 days
7. concentrationthen concentrated
8. additiondiluted in 10 mL 6 N HCl
9. concentrationconcentrated again