反应详情

33.2 g (0.2 mol) of this p-nitrobenzaldoxime, 18.3 g (0.25 mol) of boric anhydride, 1 g of a 5% Pt-C catalyst and 100 ml of methanol were charged into a hermetically sealed glass container and vigorously stirred while charging hydrogen. Reaction was continued at temperatures of 25° C. to 30° C. for 13.5 hours and 22.2 l of hydrogen was absorbed. Next, this reaction mixture was filtered to remove the catalyst and methanol was distilled off by concentration under reduced pressure. A yellow viscous liquid thus obtained was neutralized by adding 57 g (0.5 mol) of a 35% aqueous solution of sodium hydroxide and then, the liquid was separated to two layers. The lower layer, a colorless and transparent aqueous solution of sodium borate was removed and then, a brown and oily crude p-aminobenzylamine was obtained. This crude p-aminobenzylamine was subject to vacuum distillation at pressure of 5 to 6 mmHg and 22.5 g of fractions between 129.5° C. and 130° C. was obtained (yield 92.1%). The purity by means of gas chromatography was 99.93%.

1. customReaction
2. custom22.2 l of hydrogen was absorbed
3. filtrationNext, this reaction mixture was filtered
4. customto remove the catalyst and methanol
5. distillationwas distilled off by concentration under reduced pressure
6. customA yellow viscous liquid thus obtained
7. customthe liquid was separated to two layers
8. customThe lower layer, a colorless and transparent aqueous solution of sodium borate was removed