HCID 14834673、化合物 → 2,4,5-Trifluoro-3-methylaniline

HRID 232645ノート

反応式

HRID 232645 の反応式
[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]

参加物

4

反応物 1

HCID 14834673HCID 14834673、化合物

生成物 1

HCID 146512532,4,5-Trifluoro-3-methylaniline収率 77.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-664c5e0b6ed94c92a78b6c550119d3bf
出典データセット
uspto-grants-1997_01
特許番号
US05591744

反応ノート

読み込み中…