反应详情

The crude 2-(5-pyrimidinyl)-2-propylisocyanate was treated with a mixture of 1.0N sodium hydroxide (26 mL), water (20 mL) and THF (100 mL) at 0° C. for 30 min, then the mixture was poured into ethyl acetate (200 mL) and water (100 mL). The aqueous layer was acidified to pH 5 with 10% citric acid, extracted twice with ethyl acetate, and then adjusted to pH 11, saturated with sodium chloride, and extracted with methylene chloride (3×250 mL). The combined methylene chloride extracts were dried (Na2SO4) and concentrated in vacuo to give 2-(5-pyrimidinyl)-2-propylamine (950 mg) as a colorless oil.

1. extractionextracted twice with ethyl acetate
2. extractionextracted with methylene chloride (3×250 mL)
3. dry with materialThe combined methylene chloride extracts were dried (Na2SO4)
4. concentrationconcentrated in vacuo