US 12,187,693 B2
Rapid synthesis method for biomass-based amine
Hu Li, Nanjing (CN); Zhen Fang, Nanjing (CN); and Richard Lee Smith, Nanjing (CN)
Assigned to NANJING AGRICULTURAL UNIVERSITY, Jiangsu (CN)
Appl. No. 17/266,824
Filed by NANJING AGRICULTURAL UNIVERSITY, Jiangsu (CN)
PCT Filed Jul. 31, 2019, PCT No. PCT/CN2019/098614
§ 371(c)(1), (2) Date Feb. 8, 2021,
PCT Pub. No. WO2020/029846, PCT Pub. Date Feb. 13, 2020.
Claims priority of application No. 201810885588.1 (CN), filed on Aug. 6, 2018.
Prior Publication US 2021/0347750 A1, Nov. 11, 2021
Int. Cl. C07D 307/52 (2006.01); C07C 213/02 (2006.01); C07C 231/08 (2006.01)
CPC C07D 307/52 (2013.01) [C07C 213/02 (2013.01); C07C 231/08 (2013.01)] 5 Claims
 
1. A rapid synthesis method for an amine, comprising: by using formamide as an amine source, using formic acid as a hydrogen source, and using an aldehyde or ketone compound as a raw material, carrying out a direct addition reaction on the formamide and the aldehyde or ketone compound through microwave-assisted heating and in the absence of a solvent and a catalyst, and then carrying out formic acid reduction to obtain a corresponding formamide derivative; dissolving the formamide derivative in methanol, and under the action of a base, carrying out a reaction at 60 to 100° C. for 2 to 8 h to obtain the amine, wherein
the formamide derivative is prepared in a microwave reactor, a reaction system is an airtight system, nitrogen is introduced before a reaction until pressure is 1 to 3 MPa, a reaction temperature is 160 to 200° C., and a reaction time is 2 to 15 min,
a ratio of amounts of substance of the formamide, the formic acid, and the aldehyde or ketone is 6-15:6-15:2, and
the aldehyde or ketone compound is furfural, 5-methylfurfural, benzaldehyde, veratraldehyde, cinnamaldehyde, glycolaldehyde, propionaldehyde, methyl isobutyl ketone, cyclopentanone, cyclohexanone, or acetophenone.