HCID 14834673, 화합물 → 2,4,5-Trifluoro-3-methylaniline

HRID 232645노트

반응식

HRID 232645 반응식
[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([N+:9]([O-])=O)=[C:4]([F:12])[C:3]=1[CH3:13]>[Pd].C(O)(=O)C>[F:12][C:4]1[C:3]([CH3:13])=[C:2]([F:1])[C:7]([F:8])=[CH:6][C:5]=1[NH2:9]

참가 물질

4

반응물 1

HCID 14834673HCID 14834673, 화합물

생성물 1

HCID 146512532,4,5-Trifluoro-3-methylaniline수율 77.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 176Acetic Acid용매

실험 절차

To acetic acid (350 ml) are added 5% Pd-C (3.5 g) and 2,3,6-trifluoro-5-nitrotoluene (35 g) and the mixture is subjected to catalytic reduction at room temperature under atomospheric pressure. 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 obtained residue is distilled under reduced pressure to give 2,4,5-trifluoro-3-methylaniline (22.86 g), as yellow crystals, b.p. 85° C./20 mmHg.

후처리

  1. customis subjected to catalytic reduction at room temperature under atomospheric pressure
  2. filtration5% 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 obtained residue is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-664c5e0b6ed94c92a78b6c550119d3bf
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591744

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