反应详情

A mixture of lithium 2-methyl-2-(5-pyrimidinyl)propionate (4.11 g), diphenylphosphoryl azide (13.2 g), triethylamine (4.86 g) and anhydrous tert-butyl alcohol (100 mL) was heated to reflux for 6 h, then allowed to cool and concentrated in vacuo. The residue was partitioned between chloroform (250 mL) and water (100 mL), and the chloroform was extracted, dried (MgSO4) and evaporated under reduced pressure. Chromatography on silica gel, eluting with chloroform; 5% methanol gave a partially purified sample of 2-(5-pyrimidinyl)-2-propylisocyanate as a colorless oil.

1. temperaturewas heated
2. temperatureto reflux for 6 h
3. temperatureto cool
4. concentrationconcentrated in vacuo
5. customThe residue was partitioned between chloroform (250 mL) and water (100 mL)
6. extractionthe chloroform was extracted
7. dry with materialdried (MgSO4)
8. customevaporated under reduced pressure
9. washChromatography on silica gel, eluting with chloroform