反应详情

A mixture of 1-cyano-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester (89 mg, 0.33 mmol), glycine (375 mg, 5 mmol), and a 0.5 N solution of MeONa in MeOH (8 mL, 4 mmol) was refluxed with stirring for 48 h before it was concentrated in vacuo. The residue was dissolved in water (20 mL). The solution was washed with diethyl ether before its pH was adjusted to 2 to 3 by addition of aqueous 6 N HCl. The resulting suspension was extracted with ethyl acetate (1×30 mL). The organic phase was dried over MgSO4 and concentrated in vacuo to give the title compound as a yellowish solid (72 mg); MS-(−)-ion: M−1=270.2.

1. concentrationwas concentrated in vacuo
2. dissolutionThe residue was dissolved in water (20 mL)
3. washThe solution was washed with diethyl ether before its pH
4. additionwas adjusted to 2 to 3 by addition of aqueous 6 N HCl
5. extractionThe resulting suspension was extracted with ethyl acetate (1×30 mL)
6. dry with materialThe organic phase was dried over MgSO4
7. concentrationconcentrated in vacuo