Hydrochloric Acid → HCID 10405977, compound

Participants

Reaction Steps

4-(N-Methylphenylamino)-2-(2-methylphenylamino)-8-methoxyquinazoline (prepared as described in co-pending EP-A-88311461.3) (1.81 g, 0.0049 mol) was dissolved in dichloromethane (50 ml) and cooled to 0°-5° under nitrogen. Boron tribromide (6.25 g, 0.025 mol) was added dropwise via a syringe through a rubber septum over a period of 10 minutes Reaction was stirred 3 hours at 0°-5° and then allowed to rise to room temperature overnight. The reaction mixture was poured onto ice and the pH adjusted to ~12 with sodium hydroxide and then back to neutral with dilute HCl. The organic layer was separated, dried and evaporated to dryness. The solid residue was crystallised from methanol/water to give the title compound (0.66 g), m.p. 174°-175°.

Provenance & Evidence