Hydrochloric Acid → HCID 15616855, compound

Temperature

50 °C

To a solution of 1,4-diazabicyclo[3.2.2]nonane (2.75 g) in a mixture of tetrahydrofuran (40 ml) and water (20 ml) was added potassium cyanate (2.65 g) at ambient temperature. The mixture was adjusted to pH 5.0 with concentrated hydrochloric acid and stirred at 50° C. for 40 minutes. The mixture was poured into 50% aqueous solution of potassium hydroxide. The resulted aqueous solution was extracted with chloroform. The extract was dried over anhydrous potassium carbonate and evaporated to dryness in vacuo. The crystalline residue was recrystallized from diethyl ether to give 4-carbamoyl-1,4-diazabicyclo[3.2.2]nonane (898.5 mg).

1. extractionThe resulted aqueous solution was extracted with chloroform
2. dry with materialThe extract was dried over anhydrous potassium carbonate
3. customevaporated to dryness in vacuo
4. customThe crystalline residue was recrystallized from diethyl ether

ORD record

ord-95a7d3b8e6c843a0b83bd0161fc9f245

Source dataset

uspto-grants-1992_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05104866