2-Methyl-4-methoxy-5-nitrophenyl mesylate → 2-Methyl-4-methoxy-5-aminophenyl mesylate

HRID 2050755ノート

反応式

HRID 2050755 の反応式
[S:1]([O:5][C:6]1[CH:11]=[C:10]([N+:12]([O-])=O)[C:9]([O:15][CH3:16])=[CH:8][C:7]=1[CH3:17])(=[O:4])(=[O:3])[CH3:2]>[Pd].C(O)C>[S:1]([O:5][C:6]1[CH:11]=[C:10]([NH2:12])[C:9]([O:15][CH3:16])=[CH:8][C:7]=1[CH3:17])(=[O:4])(=[O:3])[CH3:2]

参加物

4

反応物 1

HCID 198211562-Methyl-4-methoxy-5-nitrophenyl mesylate

生成物 1

HCID 198211482-Methyl-4-methoxy-5-aminophenyl mesylate収率 81%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

1.55 g of 10% palladium-on-carbon, 18.8 g (71.9 mmol) of 2-methyl-4-methoxy-5-nitrophenyl mesylate and 120 ml of ethanol were fed into an autoclave (200 ml), and the mixture was then hydrogenated at 50° C. under 50 g/cm2 for 1 hours with stirring. After allowing to cool, palladium-on-carbon was filtered off and the solvent was distilled off under reduced pressure to obtain brown crystals. The crystals thus obtained were recrystallized from ethanol to thereby give 13.4 g (58.2 mmol) of 2-methyl-4-methoxy-5-aminophenyl mesylate in the form of yellow needle-like crystals. The yield was 81%.

後処理

  1. temperatureto cool
  2. filtrationpalladium-on-carbon was filtered off
  3. distillationthe solvent was distilled off under reduced pressure
  4. customto obtain brown crystals
  5. customThe crystals thus obtained
  6. customwere recrystallized from ethanol

出典と根拠

ORDレコード
ord-77587ef761f2413b87b0ad0b5b93cefb
出典データセット
uspto-grants-1991_05
特許番号
US05015260

反応ノート

読み込み中…