Methanol → 3-methoxy-N1-(3-methoxypropyl)benzene-1,2-diamine

HRID 1096626ノート

反応式

HRID 1096626 の反応式
[CH3:1][O:2][C:3]1[C:4]([N+:15]([O-])=O)=[C:5]([CH:12]=[CH:13][CH:14]=1)[NH:6][CH2:7][CH2:8][CH2:9][O:10][CH3:11].CO>[Zn].C(O)(=O)C>[CH3:1][O:2][C:3]1[CH:14]=[CH:13][CH:12]=[C:5]([NH:6][CH2:7][CH2:8][CH2:9][O:10][CH3:11])[C:4]=1[NH2:15]

参加物

5

反応物 2

HCID 887MethanolHCID 667850723-methoxy-N-(3-methoxypropyl)-2-nitroaniline

生成物 1

HCID 667862403-methoxy-N1-(3-methoxypropyl)benzene-1,2-diamine

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

Into a 100 mL round bottomed flask was added 3-methoxy-N-(3-methoxypropyl)-2-nitroaniline (36A) (560 mg, 2.33 mmol) and methanol (46 mL). Zinc metal (2.11 g, 32.4 mmol) and acetic acid (2.0 mL) was added and the mixture was stirred at room temperature for 5 hr. The mixture was filtered through a fritted Buchner funnel and the solvent was removed under vacuum. Ethyl acetate (100 mL) was added and the precipitate was filtered through a Buchner funnel with a pad of Celite. The filtrate was concentrated under vacuum to leave 3-methoxy-N1-(3-methoxypropyl)benzene-1,2-diamine (37B) as a yellow oil which was used without further purification. ESI-MS:mlz 211.4 (M-F1-1)+.

後処理

  1. filtrationThe mixture was filtered through a fritted Buchner funnel
  2. customthe solvent was removed under vacuum
  3. additionEthyl acetate (100 mL) was added
  4. filtrationthe precipitate was filtered through a Buchner funnel with a pad of Celite
  5. concentrationThe filtrate was concentrated under vacuum

出典と根拠

ORDレコード
ord-a8267ede6e3f4da99bb01b9fd023a216
出典データセット
uspto-grants-2012_03
特許番号
US08138168B1

反応ノート

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