Hydrochloric Acid → HCID 235708, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of estrone (11, 5.40 g, 20 mmol) in EtOH (100 mL) and benzene (60 mL) were added paraformaldehyde (0.600 g, 20 mmol) and N,N,N',N'-tetramethyldiaminomethane (5.5 mL, 40 mmol), and stirred for 20 h at 80° C. After the reaction mixture was cooled to 0° C., 5 N HCl was added. The aqueous layer was washed with Et2O, and basified with aqueous NH4OH. The precipitate was collected by filtration and washed with H2O, and recrystallized from EtOH to afford 4.37 g of 72 (67% yield) mp: 172-173° C.

Provenance & Evidence