Hydrochloric Acid → HCID 22763944, compound

Participants

Reaction Steps

3.27 grams of 1-bromo-3,5-di-n-butyl-adamantane were warmed with 1.2 grams of urea for 160 minutes at 165° C. The heating was performed in a closed vessel in a thermostatically controlled oil bath. After cooling, the reaction product was suspended in 50 ml. water. The water phase was brought to a pH of about 4 through dropwise addition of concentrated hydrochloric acid. The water phase was then extracted with two 10-ml. portions of ether, and brought to a pH of about 13 by dropwise addition of sodium hydroxide. The alkaline solution was stirred for about 10 minutes, after which the aqueous alkaline phase was extracted with four 10-ml. portions of benzene. The combined benzene extracts were dried over fused potassium sulfate. 1-amino-3,5-di-n-butyl-adamantane hydrochloride was precipitated by exposure to dried hydrogen chloride gas. Yield: 1.86 grams (62% of the theoretical yeild).

Provenance & Evidence