反应详情

A mixture of 4-Hydroxy-7-phenylsulfanyl-isoquinoline-3-carboxylic acid butyl ester (177 mg, 0.5 mmol; see example D-1 f), N,N-dimethylmethyleneammonium iodide (94 mg, 0.5 mmol), K2CO3 (104 mg, 0.75 mmol), and anhydrous CH2Cl2 (3 ml) was stirred at ambient temperature for 2.5 d before the mixture was concentrated in vacuo. To the residue was added water (15 ml), the mixture was acidified by addition of 6 N HCl and then washed with Et2O (3×30 ml). Subsequently, the mixture was neutralized by the addition of concentrated aqueous NaHCO3 and extracted with EtOAc (20 ml). The organic phase was dried over MgSO4 and concentrated in vacuo to give the title compound as a dark oil (34 mg); MS-(+)-ion M+1=411.1.

1. concentrationwas concentrated in vacuo
2. additionTo the residue was added water (15 ml)
3. additionthe mixture was acidified by addition of 6 N HCl
4. washwashed with Et2O (3×30 ml)
5. additionSubsequently, the mixture was neutralized by the addition of concentrated aqueous NaHCO3
6. extractionextracted with EtOAc (20 ml)
7. dry with materialThe organic phase was dried over MgSO4
8. concentrationconcentrated in vacuo