Hydrochloric Acid → N-Cyclopropyl-3-(2-(cyclopropylmethyl)-4-((2-(dimethylamino)ethoxy)methyl)-1-oxo-1,2-dihydroisoquinolin-6-yl)-4-methylbenzamide

A solution of the product of step i) (130 mg) in dichloromethane (5 mL) was treated with (−/+)-10-camphorsulfonic acid (680 mg) and N,N-dimethylethanolamine (0.32 mL) and stirred at room temperature for 17 hours. 4N Hydrogen chloride in 1,4-dioxane (0.85 mL) was added and the reaction was stirred at room temperature for 6 hrs. Additional N,N-dimethylethanolamine (0.33 mL), (−/+)-10-camphorsulfonic acid (680 mg) and 4N hydrogen chloride in 1,4-dioxane (0.9 mL) were added and the reaction was stirred at room temperature for 60 hours. The reaction mixture was diluted with dichloromethane (100 mL) and washed with saturated sodium bicarbonate (100 mL) solution. The organics were evaporated in vacuo, and the crude product was purified by HPLC to yield the title compound as a solid (25.0 mg).

1. stirringthe reaction was stirred at room temperature for 6 hrs
2. stirringthe reaction was stirred at room temperature for 60 hours
3. washwashed with saturated sodium bicarbonate (100 mL) solution
4. customThe organics were evaporated in vacuo
5. customthe crude product was purified by HPLC

ORDレコード

ord-418a1ea5769047d79af4b6f74816bb9b

出典データセット

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08012979B2