Acetic Acid → HCID 19711231、化合物

HRID 724871ノート

反応式

HRID 724871 の反応式
[NH2:1][C:2]1[C:7]2[O:8][CH2:9][CH2:10][O:11][C:6]=2[C:5]([C:12]([O:14][CH3:15])=[O:13])=[CH:4][C:3]=1[N+:16]([O-])=O.C(O)(=O)C>C(O)C.[Pd]>[NH2:16][C:3]1[CH:4]=[C:5]([C:12]([O:14][CH3:15])=[O:13])[C:6]2[O:11][CH2:10][CH2:9][O:8][C:7]=2[C:2]=1[NH2:1]

参加物

5

反応物 2

HCID 176Acetic AcidHCID 19711229HCID 19711229、化合物

生成物 1

HCID 19711231HCID 19711231、化合物収率 92%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

A stirred suspension of methyl 8-amino-7-nitro-1,4-benzodioxan-5-carboxylate (300 mg, 0.0012 mole) in ethanol (30 ml) together with glacial acetic acid (5 ml) was hydrogenareal over 10% Pd-C (100 mg) at atmospheric pressure and temperature for 5 h. The catalyst was filtered off and the filtrate concentrated in vacuo. The residue was basified with concentrated potassium carbonate solution and extracted with ethyl acetate. The extract was dried (Na2SO4) and concentrated in vacuo to afford methyl 7,8-diamino-1,4-benzodioxan-5-carboxylate as a beige solid (240 mg, 92%). 1H NMR (CDCl3) δ:6.91(s,1 H), 4.21(s,4 H), 3.96(br s.2 H), 3.74(s,3 H), 3.0(br s,2 H).

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate concentrated in vacuo
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried (Na2SO4)
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-cffc758317bd4280ba76d75e86c2e51f
出典データセット
uspto-grants-1998_01
特許番号
US05705509

反応ノート

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