PURIFICATION OF 4-CYANOQUINUCLIDINE SULFURIC ACID ADDUCT

摘要

PURPOSE:To enable to readily obtain a compound useful as an intermediate for drugs in high purity and in a good yield by mixing 4-cyanoquinuclidine with concentrated sulfuric acid and subsequently with methanol, etc., to deposit crystals. CONSTITUTION:A substance to be purified containing 4-quinuclidine or a salt thereof is reacted with concentrated sulfuric acid at -10 to 50 deg.C for 30 min to 24 hr to obtain 4-cyanoquinuclidine sulfuric acid adduct. The reaction solution is mixed with methanol and some other alcohol (ethanol) at a temperature of =35 deg.C to deposit the highly pure crystals of the objective compound. 1 Mole of 4-cyanoquinuclidine is mixed with 2-10 moles of concentrated sulfuric acid and 50g, preferably 100-1000g, of methanol, etc. The subjection of the 4- cyanoquinuclidine sulfuric acid adduct only to a neutralization reaction permits to lead to 4-carbamoyl quinuclidine.