Sodium Chloride → HCID 67253910, compound

Participants

Reaction Conditions

Reaction Steps

To 353 mg (0.96 mmol) of N-[3-(2-chloro-6,7-dimethoxyquinazolin-4-yl)phenyl]acetamide, tetrahydrofuran (2.06 mL), and methanol (1.03 mL) was added a methanol solution (2.06 mL) of 40% methylamine, and the mixture was reacted at 90° C. for 9 hours. The mixture was allowed to cool and then poured into a mixed solution of ethyl acetate (30 mL) and 5% w/w sodium chloride solution (30 mL) while washing with tetrahydrofuran (30 mL) to extract the organic layer. The organic layer was washed with 5% w/w sodium chloride solution (30 mL) and then concentrated under reduced pressure. To the concentration residue was added t-butyl methyl ether (3 mL), and the mixture was crystallized with a spatula and then suspended by stirring at 50° C. for 2 hours. The mixture was allowed to cool gradually, and then the precipitated crystals were collected by filtration and dried to give 318 mg of a target product (yield: 91.1%).

Provenance & Evidence