反应详情

A mixture of the crude 1′-(8-chloro-5,6-dihydro-4H-[1,2,4]triazolo[4,3-a][1,4]benzodiazepin-1-yl)-1H-spiro[isochromene-4,4′-piperidine] (0.10 g, 0.24 mmol) and paraformaldehyde (0.057 g, 1.9 mmol) in methanol (2 ml) was heated at reflux for 4 h. After cooling to room temperature sodium cyanoborohydride (0.03 g, 0.47 mmol) was added at 0° C. The reaction mixture was allowed to warm to room temperature and stirred for 18 h. Quenching with 1 M aqueous sodium hydroxide solution (30 ml) was followed by extraction with ethyl acetate.

1. temperaturewas heated
2. temperatureat reflux for 4 h
3. additionwas added at 0° C
4. customQuenching with 1 M aqueous sodium hydroxide solution (30 ml)
5. extractionwas followed by extraction with ethyl acetate