Triethylamine → 2-(6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)-N-[1-{3'-[(ethylsulfonyl)amino]-4-biphenylyl}-2-(4-morpholinyl)ethyl]-N-methylacetamide

To a solution of N-[1-(3′-amino-4-biphenylyl)-2-(4-morpholinyl)ethyl]-2-(6,7-dichloro-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)-N-methylacetamide (70.1 mg, 0.12 mmol) in dichloromethane (1 mL) was added ethanesulfonyl chloride (32 mg, 0.24 mmol). Triethylamine (50 mg, 0.50 mmol) was added and the resultant mixture was stirred at room temperature for 16 h. The mixture was concentrated under reduced pressure and the residue was purified by Gilson preparative HPLC (Sunfire Prep C18, 30×150 mm, 50 mL/min, A: acetonitrile with 0.1% TFA B: water with 0.1% TFA, A: 30 to 60% over 12 min, UV detection at 214 nm) to give 26.4 mg (33%) of the title compound as off white solid. MS (ES) m/e 661.2 [M+H]+.

1. concentrationThe mixture was concentrated under reduced pressure
2. customthe residue was purified by Gilson preparative HPLC (Sunfire Prep C18, 30×150 mm, 50 mL/min

ORDレコード

ord-b504a9880c484ff4a6d3e591249f7dc4

出典データセット

uspto-grants-2008_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07432258B2