Formic Acid → 2-Nitrobenzene-1,3-diamine

Temperature

90 °C

68 mg of palladium at a concentration of 10% on charcoal are added to 0.016 mole (3 g) of 4-chloro-2,6-diaminonitro-benzene in 6 ml of triethylamine, and 1.32 ml of formic acid are then added dropwise. A high exothermicity is noted. The reaction medium is heated to 90° C. for 1 hour 30. After dilution of the reaction mixture with ethanol, the catalyst is removed by hot filtration. The filtrate, evaporated to dryness under reduced pressure, enables a dry extract to be obtained. After dilution of the dry extract with water, the expected product precipitates. After filtration and washing with water, followed by drying under vacuum in the presence of phosphorus pentoxide, it is recrystallized from toluene. It melts at 142° C. (literature 141° C., 145° C.).

1. additionare then added dropwise
2. customAfter dilution of the reaction mixture with ethanol, the catalyst is removed by hot filtration
3. customThe filtrate, evaporated to dryness under reduced pressure
4. extractionextract
5. customto be obtained
6. extractionAfter dilution of the dry extract with water
7. customthe expected product precipitates
8. filtrationAfter filtration
9. washwashing with water
10. dry with materialby drying under vacuum in the presence of phosphorus pentoxide, it
11. customis recrystallized from toluene
12. customIt melts at 142° C. (literature 141° C., 145° C.)

ORD record

ord-2d58795f0f45483ab6f6697622e6a4c0

Source dataset

uspto-grants-1991_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04992586