反应详情

A warm solution of 2.5 gm. (0.014 mole) of 2-chloro-6-nitrobenzaldehyde in 40 ml. of alcohol 3A was added, with stirring, to a warm solution of 1.5 gm. (0.014 equivs.) of carboxymethoxylamine hemihydrochloride and 1.7 gm. (0.021 equiv.) of anhyd. sodium acetate in 40 ml. of water. The reaction mixture was heated a half-hour on the steam bath, and was then evaporated to a volume of about 20 ml. A solid separated upon cooling; it was filtered from the mixture, washed with cold water and dried in air to give 2.7 gm. (77.3%) of tan-yellow colored material melting at 136°-141° C. Recrystallization from n-hexane/isopropyl alcohol yield 2.5 gm. of pale tan-yellow crystalline product melting at 144°-146° C.

1. temperatureThe reaction mixture was heated a half-hour on the steam bath
2. customwas then evaporated to a volume of about 20 ml
3. customA solid separated
4. temperatureupon cooling
5. filtrationit was filtered from the mixture
6. washwashed with cold water
7. customdried in air
8. customto give 2.7 gm
9. customRecrystallization from n-hexane/isopropyl alcohol yield 2.5 gm