反应详情

A solution of 5.6 g of ethyl 2-{[(1-carbamoyl-1,2-dimethylpropyl)amino]methyl}-5-ethylnicotinate (0.0174 mol) in 30 mL of methanol containing 2 g of NaOH (0.05 mol) and 10 mL water is stirred at room temperature for two hours and 30 minutes. The reaction is concentrated in vacuo and redissolved in 30 mL water; adjustment of the pH to 4 with concentrated hydrochloric acid and concentration in vacuo gives a gum. This residue is dissolved in a mixture of ethyl acetate, tetrahydrofuran, and methanol, dried over MgSO4, and concentrated in vacuo to 6 g foam. Crystallization from methanol-ether affords 3.1 g product, mp 180°-181° C.

1. concentrationThe reaction is concentrated in vacuo
2. dissolutionredissolved in 30 mL water
3. concentrationadjustment of the pH to 4 with concentrated hydrochloric acid and concentration in vacuo
4. customgives a gum
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo to 6 g foam
7. customCrystallization from methanol-ether