Ethyl Acetate → Methyl 6-amino-1,3-benzodioxole-5-carboxylate

HRID 1598978

反応式

HRID 1598978 の反応式
[N+:1]([C:4]1[C:5]([C:13]([O:15][CH3:16])=[O:14])=[CH:6][C:7]2[O:11][CH2:10][O:9][C:8]=2[CH:12]=1)([O-])=O.C(OCC)(=O)C>[Pd].CO>[NH2:1][C:4]1[C:5]([C:13]([O:15][CH3:16])=[O:14])=[CH:6][C:7]2[O:11][CH2:10][O:9][C:8]=2[CH:12]=1

参加物

5

反応物 2

HCID 8857Ethyl AcetateHCID 697581,3-Benzodioxole-5-carboxylic acid, 6-nitro-, methyl ester

生成物 1

HCID 290838Methyl 6-amino-1,3-benzodioxole-5-carboxylate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A mixture of the methyl 6-nitro-1,3-benzodioxole-5-carboxylate, 5% palladium on carbon (1.5 g), ethyl acetate (180 mL) and methanol (80 mL) was stirred 3 hours under a hydrogen atmosphere (15 psi). The mixture was filtered and concentrated and the residue was recrystallized from cyclohexane (200 mL) to give methyl 6-amino-1,3-benzodioxole-5-carboxylate (6.3 g, 32 mmol), m.p. 107°-108° C.

後処理

  1. filtrationThe mixture was filtered
  2. concentrationconcentrated
  3. customthe residue was recrystallized from cyclohexane (200 mL)

出典と根拠

ORDレコード
ord-8ccdd3dd60c04b8cbabf949a05640412
出典データセット
uspto-grants-1998_04
特許番号
US05739336

関連ノート

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