反应详情

7.1 g. 4-Nitroxypiperidine are dissolved in 60 ml. water and 30 ml. methanol and mixed with 16.2 g. potassium cyanate. After the dropwise addition of 12 ml. glacial acetic acid, stirring is continued at ambient temperature for 4 hours. The inorganic salts are precipitated out by the addition of 100 ml. ethyl acetate. After suction filtration, the aqueous phase is separated off and the organic phase is dried with anhydrous sodium sulphate. After suction filtration, the filtrate is evaporated in a vacuum. The residue is triturated with diethyl ether and the crystals are filtered off with suction. There are obtained 8.3 g. of the title compound, i.e. 89% of theory; m.p. 110°-111° C.

1. additionAfter the dropwise addition of 12 ml
2. customThe inorganic salts are precipitated out by the addition of 100 ml
3. filtrationAfter suction filtration
4. customthe aqueous phase is separated off
5. dry with materialthe organic phase is dried with anhydrous sodium sulphate
6. filtrationAfter suction filtration
7. customthe filtrate is evaporated in a vacuum
8. customThe residue is triturated with diethyl ether
9. filtrationthe crystals are filtered off with suction
10. customThere are obtained 8.3 g