反应详情

7.9 g of m-cyanobenzylamine, 8.4 g of hexamethylenetetramine, 40 ml of water and 40 ml of acetic acid were mixed and reacted at 104° C. for 2 hours while stirring. The reaction solution was cooled to room temperature and thereto 12 g of concentrated sulfuric acid was added. The solvent was concentrated to dry in an evaporator with a water bath at 70° C. The concentration residue was separated by toluene/water and washed with water. The toluene layer obtained was concentrated until crystals were precipitated. The concentrated toluene solvent was placed in water and after removing toluene by azeotropic distillation, the residue was cooled to room temperature. The crystals precipitated were collected by filtration, washed with water and dried to obtain 5.9 g (yield: 74%) of m-cyanobenzaldehyde. The purity was 99% or more.

1. customreacted at 104° C. for 2 hours
2. concentrationThe solvent was concentrated
3. customto dry in an evaporator with a water bath at 70° C
4. customThe concentration residue was separated by toluene/water
5. washwashed with water
6. customThe toluene layer obtained
7. concentrationwas concentrated until crystals
8. customwere precipitated
9. customafter removing toluene
10. distillationby azeotropic distillation
11. temperaturethe residue was cooled to room temperature
12. customThe crystals precipitated
13. filtrationwere collected by filtration
14. washwashed with water
15. customdried