反应详情

20.9 g (75.0 mmol) of N-[2-hydroxy-3-(1-piperidinyl)propoxy]-3-pyridine-carboximidamide [Hung. Pat. 177.578 (1976)] was dissolved in 300 ml of benzene. To this solution 150 ml of 1 N sodium hydroxide solution was added, followed by dropwise addition of 19.5 ml (168 mmol) of benzoyl chloride. After stirring the mixture intensively for 2 hours, 7.1 g (67 mmol) of sodium carbonate and a further portion of benzoyl chloride (9.75 ml; 84 mmol) was added, and the stirring was continued overnight. The phases were then separated, the organic layer was extracted with 1 N sodium hydroxide solution and water, dried and evaporated to dryness. The residue (41 g oil) was dissolved in 150 ml of acetone, and 8.7 g (75 mmol) maleic acid was added. The obtained precipitate was filtered off, washed with acetone, and dried.

1. waitthe stirring was continued overnight
2. customThe phases were then separated
3. extractionthe organic layer was extracted with 1 N sodium hydroxide solution and water
4. customdried
5. customevaporated to dryness
6. dissolutionThe residue (41 g oil) was dissolved in 150 ml of acetone
7. filtrationThe obtained precipitate was filtered off
8. washwashed with acetone
9. customdried