Methanol → 2-(S)-{[7-(4-Fluoro-phenoxy)-4-hydroxy-1-methyl-isoquinoline-3-carbonyl]-amino}-propionic acid

A mixture of 7-(4-Fluoro-phenoxy)-4-hydroxy-1-methyl-isoquinoline-3-carboxylic acid butyl ester (92 mg, 0.25 mmol), (S)-alanine (225 mg, 2.5 mmol) and a 0.5 N solution of MeONa in MeOH (5 ml, 2.5 mmol) was heated in a microwave oven with stirring for 20 min at 140° C. before the mixture was concentrated in vacuo. To the residue was added water (10 ml) and the mixture was washed with EtOAc (2×25 ml). The so purified aq. solution was acidified by the addition of 6 N HCl and extracted with EtOAc (1×25 ml). The organic phase was dried over MgSO4 and concentrated in vacuo to give the title compound as a tan solid (69 mg); MS-(+)-ion M+1=385.1.

1. concentrationwas concentrated in vacuo
2. additionTo the residue was added water (10 ml)
3. washthe mixture was washed with EtOAc (2×25 ml)
4. customThe so purified aq. solution
5. additionwas acidified by the addition of 6 N HCl
6. extractionextracted with EtOAc (1×25 ml)
7. dry with materialThe organic phase was dried over MgSO4
8. concentrationconcentrated in vacuo

ORDレコード

ord-248af5634ec14dedbc96f2049107e76e

出典データセット

uspto-grants-2009_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07629357B2