反应详情

BH3.SMe2 (1.36 mL, 5.0 M in Et2O, 6.8 mmol) was added to solution of methyl4-[(9-cyclopentyl-5-methyl-6-oxo-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-yl)amino]-3-methoxybenzoate (Intermediate 8; 290 mg, 0.68 mmol) in THF (4 mL) and stirred for 5 h at ambient temperature under an atmosphere of nitrogen. HCl (10 mL, concentrated aqueous) was added and the resulting solution was stirred at ambient temperature for 16 h. The HCl solution was then diluted with water (50 mL), and loaded onto an SCX-2 column. The SCX-2 column was then washed with water (50 mL) and MeOH (50 mL). The product was then eluted from the SCX-2 column with NH3 (50 mL, 7M in MeOH). The volatiles were then removed under reduced pressure to afford the title compound (250 mg, 89%) as a solid.

1. additionwas added
2. stirringthe resulting solution was stirred at ambient temperature for 16 h
3. washThe SCX-2 column was then washed with water (50 mL) and MeOH (50 mL)
4. washThe product was then eluted from the SCX-2 column with NH3 (50 mL, 7M in MeOH)
5. customThe volatiles were then removed under reduced pressure