Hydrochloric Acid → HCID 19957051, compound

Participants

Reaction Steps

To a mixture of 4,5-dihydro-1-(4-methoxyphenyl)-4-methyl-3-[2-(4-pyridyl)ethyl]-1H-2,4-benzodiazepine dihydrochloride (3.81 g, 8.6 mmol, prepared from the fumarate of Example 398 by standard procedures) in CH2Cl2 (40 mL) in an ice-bath under N2 was added boron tribromide (17.2 mL, 1M in CH2Cl2). The mixture was stirred for 3 hours, 2N HCl was added and the mixture was stirred for 1/2 hour. The layers were separated, the aqueous layer was extracted with CH2Cl2 and the combined organic layers were washed with 2N HCl. The organic layer was treated with saturated Na2CO3 and the product which precipitates was collected by filtration to afford 3.06 g (83%) of 4,5-dihydro-1-(4-hydroxyphenyl)-4-methyl-3-[2-(4-pyridyl)ethyl]-1H-2,4-benzodiazepine dihydrochloride, m.p. 258°-259° C. after recrystallization from methanol/ether.

Provenance & Evidence