反应详情

2.26 g (10.7 mmol) of the compound from Example IV are boiled under reflux with 3.48 g (53.6 mmol) of sodium azide and 7.37 g (53.6 mmol) of triethylammonium chloride in 30 ml of analytical grade dimethylformamide for 24 hours. After cooling, the mixture is partitioned between ether and 1M sulphuric acid, the organic phase is washed with water and dried over sodium sulphate and the solvent is evaporated off. The crude product is extracted by stirring in toluene and, after filtration with suction, the product is dried in vacuo (1.89 g, 7.2 mmol). The mother liquor is evaporated on a rotary evaporator and the residue is purified again as above (0.43 g, 1.7 mmol).

1. temperatureAfter cooling
2. customthe mixture is partitioned between ether and 1M sulphuric acid
3. washthe organic phase is washed with water
4. dry with materialdried over sodium sulphate
5. customthe solvent is evaporated off
6. extractionThe crude product is extracted
7. filtrationafter filtration with suction
8. customthe product is dried in vacuo (1.89 g, 7.2 mmol)
9. customThe mother liquor is evaporated on a rotary evaporator
10. customthe residue is purified again as above (0.43 g, 1.7 mmol)