Ammonium formate → 1-Tert-butyl-2-methoxy-5-(trifluoromethyl)-4-aminobenzene

HRID 1915337ノート

反応式

HRID 1915337 の反応式
[C:1]([C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:13])[F:12])[C:8]([N+:15]([O-])=O)=[CH:7][C:6]=1[O:18][CH3:19])([CH3:4])([CH3:3])[CH3:2].C([O-])=O.[NH4+]>CCO.[Pd]>[C:1]([C:5]1[CH:10]=[C:9]([C:11]([F:14])([F:12])[F:13])[C:8]([NH2:15])=[CH:7][C:6]=1[O:18][CH3:19])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 574702461-Tert-butyl-2-methoxy-5-(trifluoromethyl)-4-nitrobenzene

生成物 1

HCID 574702471-Tert-butyl-2-methoxy-5-(trifluoromethyl)-4-aminobenzene収率 95.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

To a refluxing solution of 1-tert-butyl-2-methoxy-5-(trifluoromethyl)-4-nitrobenzene (473 mg, 1.7 mmol) and ammonium formate (473 mg, 7.3 mmol) in EtOH (10 mL) was added 10% Pd—C (200 mg). The mixture was refluxed for 1 h, cooled and filtered through Celite. The solvent was removed by evaporation to give 1-tert-butyl-2-methoxy-5-(trifluoromethyl)-4-aminobenzene (C-18) (403 mg, 95%). 1H NMR (400 MHz, CDCl3) δ 7.19 (s, 1H), 6.14 (s, 1H), 4.02 (bs, 2H), 3.74 (s, 3H), 1.24 (s, 9H).

後処理

  1. temperatureThe mixture was refluxed for 1 h
  2. temperaturecooled
  3. filtrationfiltered through Celite
  4. customThe solvent was removed by evaporation

出典と根拠

ORDレコード
ord-c21ddb9ff24d4a338c319f9757b7fc10
出典データセット
uspto-grants-2013_12
特許番号
US08614327B2

反応ノート

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