2,6-Difluoro-3-nitrotoluene → 2,4-Difluoro-3-methylaniline

To acetic acid (1.2 l) are added 5% Pd-C (24 g) and 2,6-difluoro-3-nitrotoluene (238.7 g) and the mixture is subjected to catalytic reduction at room temperature under 4.5 atoms. The 5% Pd-C is filtered off and the acetic acid is distilled off under reduced pressure. The residue is poured into ice-water, neutralized, extracted with dichloromethane, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the residue is distilled under reduced pressure to give 2,4-difluoro-3-methylaniline (138 g), colorless oils, b.p.: 75° C./11 mmHg.

1. customis subjected to catalytic reduction at room temperature under 4.5 atoms
2. filtrationThe 5% Pd-C is filtered off
3. distillationthe acetic acid is distilled off under reduced pressure
4. additionThe residue is poured into ice-water
5. extractionextracted with dichloromethane
6. washthe extract is washed with water
7. customdried
8. distillationThe solvent is distilled off under reduced pressure
9. distillationthe residue is distilled under reduced pressure

ORD record

ord-b3ca1a75b8c5440280ccc45fadaaf014

Source dataset

uspto-grants-1997_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05591744