反应详情

温度

0 °C

A solution of intermediate (19) (0.0302 mole) and concentrated HCl (0.0906 mole) in acetic acid (100 ml) was stirred at 0° C. A solution of NaNO2 (0.032 mole) in water (10 ml) was added dropwise at 0° C. The reaction mixture was stirred for 1 hour at 0° C. A powdered mixture of sodium acetate (0.0906 mole) and diethyl(1,3-dioxo-1,3-propanediyl)biscarbamate (0.0332 mole) was added portionwise. The mixture was allowed to warm to RT and stirred for 1 hour. Water was added and this mixture was extracted with CH2Cl2. The separated organic layer was dried, filtered and the solvent evaporated, yielding diethyl N,N′-[2-[[3,5-dichloro-4-[1-[5-(2-methylphenyl)-1,2,4-oxadiazol-3-yl]-1-methylethyl]phenyl]hydrazono]-1,3-dioxo-1,3-propanediyl]dicarbamate (intermediate 20).

1. additionwas added portionwise
2. temperatureto warm to RT
3. stirringstirred for 1 hour
4. extractionthis mixture was extracted with CH2Cl2
5. customThe separated organic layer was dried
6. filtrationfiltered
7. customthe solvent evaporated