反应详情

A mixture of 56 mg (0.2 mmol) of 1-chloro-4-hydroxy-isoquinoline-3-carboxylic acid butyl ester from example B-1 c), 227 mg (2 mmol) of N-(2-amino-ethyl)-acetamide and 0.8 ml of absolute ethanol was stirred at ambient temperature for 3 days. Then the solvent was evaporated in vacuo, the residue suspended in 3 ml of water, and the pH of the mixture was adjusted 2 to 3 by the addition of aqueous 1N HCl. The mixture was extracted with 2×25 ml of ethyl acetate. The combined organic phases were dried over sodium sulfate and evaporated in vacuo to give a yellowish solid. 64 mg of the title compound were obtained; MS-(+)-ion: M+1=308.1.

1. customThen the solvent was evaporated in vacuo
2. additionby the addition of aqueous 1N HCl
3. extractionThe mixture was extracted with 2×25 ml of ethyl acetate
4. dry with materialThe combined organic phases were dried over sodium sulfate
5. customevaporated in vacuo
6. customto give a yellowish solid