Water → 3-(5-Aminopyrazin-2-yl)-N-(4-(trifluoromethoxy)phenyl)benzamide

3-Bromo-N-(4-(trifluoromethoxy)phenyl)benzamide (Stage 3.1, 50 mg, 0.139 mmol), 5-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)pyrazin-2-amine (0.180 mmol), 2 M Na2CO3 (0.104 mL, 0.208 mmol), (Ph3P)4Pd (8 mg, 6.94 μmol), water (0.8 mL) and DME (2.4 mL) were added to a vial, which was sealed and subjected to MW irradiation at 150° C. for 10 min. The RM was filtered through a PL-Thiol MP SPE cartridge (StratoSpheres™, 6 mL) and the cartridge was washed with MeOH (10 mL). The combined filtrates were evaporated to dryness under reduced pressure and the crude product was purified by preparative HPLC to afford the title compound. UPLC-MS (Condition 6) tR=1.84 min, m/z=375.3 [M+H]+.

1. customwas sealed
2. customsubjected to MW irradiation at 150° C. for 10 min
3. filtrationThe RM was filtered through a PL-Thiol MP SPE cartridge (StratoSpheres™, 6 mL)
4. washthe cartridge was washed with MeOH (10 mL)
5. customThe combined filtrates were evaporated to dryness under reduced pressure
6. customthe crude product was purified by preparative HPLC

ORDレコード

ord-4f33e558f5434e308935840b836f511a

出典データセット

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09315489B2