反应详情

温度

60 °C

7-Chloro-1-(4-methoxybenzyl)-3-(naphthalen-2-ylmethyl)-5-(1,4-dioxa-8-azaspiro[4.5]decan-8-yl)-1H-benzo[e][1,4]diazepin-2(3H)-one (0.14 g, 0.24 mmol) was dissolved in 1,4-dioxane (4 mL), and concentrated aqueous hydrochloric acid (4 mL) was added. The reaction mixture was stirred at 60° C. for 5 hours, then the temperature increased to 80° C. for 2 hours. The solution was cooled, diluted with ethyl acetate, washed with saturated sodium bicarbonate solution, brine, dried with sodium sulfate, decanted and concentrated in the presence of silica. Chromatography provided 7-chloro-3-(naphthalen-2-ylmethyl)-5-(4-oxopiperidin-1-yl)-1H-benzo[e][1,4]diazepin-2(3H)-one (22 mg, 22% yield). ESI m/z measured 432.1487 [M+H]+. calculated 432.1479.

1. temperaturethe temperature increased to 80° C. for 2 hours
2. temperatureThe solution was cooled
3. washwashed with saturated sodium bicarbonate solution, brine
4. dry with materialdried with sodium sulfate
5. customdecanted
6. concentrationconcentrated in the presence of silica