反应详情

温度

0 °C

LiOH (1.3 mmol, 0.03 g) was added to a solution of trans-4-(1-Methyl-2,4-dioxo-1,2,4,5-tetrahydro-benzo[d][1,3]diazepin-3-ylmethyl)-cyclohexane carboxylic acid methyl ester (0.84 mmol, 0.29 g) in dioxane (3 mL) and water (3 mL) at 0° C. The mixture was stirred at 0° C. for 2 h. The reaction mixture was washed with DCM, then HCl (1N) was added until reached pH 1, then extract with DCM (3×10 mL) and AcOEt (3×10 mL). The organic layers were washed with brine (2×10 mL) dried over Na2SO4 collected together and concentrated under reduced pressure to give the title compound in quantitative yield (0.29 g).

1. washThe reaction mixture was washed with DCM
2. additionHCl (1N) was added
3. extractionextract with DCM (3×10 mL) and AcOEt (3×10 mL)
4. washThe organic layers were washed with brine (2×10 mL)
5. dry with materialdried over Na2SO4
6. customcollected together
7. concentrationconcentrated under reduced pressure