反应详情

3-[5-(3-methyl-4-isothiazolyl)-2,4-dioxo-3,4-dihydro-1(2H)-pyrimidinyl]propanal (Prep 0.126 mmol) was dissolved in 1,2-Dichloroethane (DCE) (1 ml). (1S,5R)-1-[4-(trifluoromethyl)phenyl]-3-azabicyclo[3.1.0]hexane (P4, 28.6 mg, 0.126 mmol) and ACETIC ACID (0.022 ml, 0.378 mmol) were added and the mixture was stirred at rt for 15 minutes. Then it was cooled at 0° C. and SODIUM TRIACETOXYBOROHYDRIDE (29.4 mg, 0.139 mmol) was added. The mixture was stirred at 0° C. for 3 hours. The mixture was treated with NaHCO3 aqueous saturated solution (5 mL) and extracted with DCM (3×5 mL). The organic were filtered on a separatory cartridge, combined and dried to afford a crude that was submitted to LC preparative purification. Fraction collected was dried (rotary) to afford the title compound as a white solid (8.7 mg, 14% yield).

1. temperatureThen it was cooled at 0° C.
2. stirringThe mixture was stirred at 0° C. for 3 hours
3. extractionextracted with DCM (3×5 mL)
4. filtrationThe organic were filtered on a separatory cartridge
5. customdried
6. customto afford a crude that
7. customwas submitted to LC preparative purification
8. customFraction collected
9. customwas dried (rotary)