反应详情

To 2-((R)-1-amino-2-methyl-propyl)-3-benzyl-7-chloro-3H-quinazolin-4-one (1.0 g, 2.9 mMol) in DMF (10 mL) was added DIEA (0.6 mL, 3.4 mMol) and 1-toluoyloxy-3-bromopropan-2-one (1.0 g, 3.7 mMol) (Prepared using the procedure of F. C. Hartman, Biochemistry, 9, 1776 (1970) except substituting toluoyl chloride for benzoyl chloride.) The reaction was stirred at RT for 18 h, concentrated under vacuum, taken up in EtOAc, washed with 1 N Na2CO3, dried (Na2SO4) and evaporated to dryness. The product was converted to its hydrochloride salt by treating with 4 N HCl in dioxane (20 mL) and concentration under vacuum. Trituration with (1:1) Et2O/pet. ether, filtration and drying under vacuum left the title compound (1.87 g, 100%, 88% pure) as a beige solid: MS (ES) m/e 532.2 (M+H)+.

1. customPrepared
2. concentrationconcentrated under vacuum
3. washwashed with 1 N Na2CO3
4. dry with materialdried (Na2SO4)
5. customevaporated to dryness
6. additionby treating with 4 N HCl in dioxane (20 mL) and concentration under vacuum
7. filtrationTrituration with (1:1) Et2O/pet. ether, filtration
8. customdrying under vacuum
9. waitleft the title compound (1.87 g, 100%, 88% pure) as a beige solid