反应详情

24 mmol of sodium cyanoborohydride w&e added to 5 mmol of 8-methyl-1,2,3,4-tetrahydroquinoline-5-carboxylic acid and 50 mmol of paraformaldehyde in 30 ml of glacial acetic acid, the temperature of the reaction mixture being kept below 30° C. using an ice bath. The reaction mixture was stirred at room temperature for 15 hours, poured onto ice and adjusted to pH 4 with aqueous sodium hydroxide solution. The mixture was then extracted with ethyl acetate and the organic phase was washed with water, dried over sodium sulfate and concentrated.

1. custombeing kept below 30° C.
2. additionpoured onto ice
3. extractionThe mixture was then extracted with ethyl acetate
4. washthe organic phase was washed with water
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated