反应详情

5 g (27.5 mmol) of 4-Nitro-2-methoxymethyl-aminobenzene and 0.250 g of palladium (10% on carbon) are placed in a 250 ml Parr bottle and 50 g of ethyl acetate is added. Hydrogenation is carried out using a Parr apparatus under 50-60 psig (64.7-74.7 psi or 446-515 kPa) of hydrogen pressure. In the course of the reaction the yellowish grey suspension turns to a darker grey suspension. The reaction is also carefully monitored for rapid hydrogen uptake and additional hydrogen is introduced to keep pressure above 50 psig (64.7 psi or 446 kPa). After 1 hour the suspension clears, leaving a yellow solution. The reaction is continued for 2.5 hours to ensure complete conversion. The catalyst is removed by filtration through glass microfiber filter paper. The filtrate is concentrated to ca. 25 ml, and 25 ml of toluene are added to precipitate the product. The product is collected on filter paper with suction and dried at 60° C. under vacuum. The product yield is 4.5 g.

1. additionis added
2. customIn the course of the reaction the yellowish grey suspension
3. additionis introduced
4. customleaving a yellow solution
5. waitThe reaction is continued for 2.5 hours
6. customThe catalyst is removed by filtration through glass microfiber
7. filtrationfilter paper
8. concentrationThe filtrate is concentrated to ca. 25 ml, and 25 ml of toluene
9. additionare added
10. customto precipitate the product
11. customThe product is collected
12. filtrationon filter paper with suction
13. customdried at 60° C. under vacuum