Dimethylformamide → HCID 66713332, compound

200 mg I.14 was suspended in 1 mL dimethylformamide, 1 mL tetrahydrofuran and 4 mL methylamine solution (40% in water) and stirred at 40° C. overnight. The mixture was concentrated half, 20 mL water and dioxane was added and the mixture stirred at ambient temperature for 30 min. The solid was filtered off and the filtrate was concentrated. The crude was dissolved in methanol and dichloromethane and purified via chromatography (amino phase: dichloromethane/methanol 80:20) and the appropriate fractions combined and concentrated.

1. concentrationThe mixture was concentrated half, 20 mL water and dioxane
2. additionwas added
3. filtrationThe solid was filtered off
4. concentrationthe filtrate was concentrated
5. dissolutionThe crude was dissolved in methanol
6. customdichloromethane and purified via chromatography (amino phase: dichloromethane/methanol 80:20)
7. concentrationconcentrated

ORD record

ord-297ef10b5f344b77988efc3084899799

Source dataset

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08969568B2