Ammonium formate → (R)-1-(4-cyclopropyl-benzenesulfonyl)-4-(5-cyclopropyl-thiazolo[4,5-d]pyrimidin-2-yl)-piperazine-2-carboxylic acid 4-trifluoromethoxy-benzylamide

Temperature

80 °C

To a mixture of the compound (54 mg) obtained in Step 1 and ammonium formate (49 mg) in ethanol (2.0 ml) was added 10% palladium carbon (50 mg) at 80° C. After stirring at 80° C. for 30 min, ammonium formate (49 mg) and 10% palladium carbon (50 mg) were added. After stirring at 80° C. for 30 min, the reaction mixture was allowed to return to room temperature, and the reaction mixture was diluted with ethyl acetate. The mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by thin layer silica gel chromatography (ethyl acetate) to give the title compound (24 mg).

1. stirringAfter stirring at 80° C. for 30 min
2. customto return to room temperature
3. filtrationThe mixture was filtered through celite
4. concentrationthe filtrate was concentrated under reduced pressure
5. customThe residue was purified by thin layer silica gel chromatography (ethyl acetate)

ORD record

ord-4195838b1a7444858e21687bf00e30c9

Source dataset

uspto-grants-2011_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08017612B2