Formaldehyde → HCID 57979831, compound

Participants

Reaction Steps

Solid sodium triacetoxy borohydride (0.2 g, 0.94 mmol) was added to a stirred solution of N2-({4-[(3-chloro-2-fluorophenyl)amino]-7-methoxyquinazolin-6-yl}methyl)-N1,2-dimethylalaninamide (0.12 g, 0.28 mmol Example 95) in a mixture of acetic acid/dichloromethane (10 ml, 5% v/v) and in the presence of type 4 Å molecular sieves, followed rapidly by aqueous formaldehyde (1 ml). After 10 minutes the reaction mixture was concentrated and purified by preparative LCMS (standard basic system) to give the title product as a white solid, (0.085 g, 69%); 1H NMR Spectrum: (DMSO d6) 1.24 (s, 6H), 2.18 (s, 3H), 2.65 (d, 3H), 3.52 (s, 2H), 3.96 (s, 3H), 7.20 (s, 1H), 7.29 (t, 1H), 7.52-7.62 (m, 2H), 7.79 (m, 1H), 8.44 (m, 2H), 9.78 (s, 1H); Mass Spectrum: (M+H)+ 446.

Provenance & Evidence