Ammonia → 3-Methoxy-2-methylbenzamide

HRID 722778ノート

反応式

HRID 722778 の反応式
[CH3:1][O:2][C:3]1[C:4]([CH3:12])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6](O)=[O:7].C1C=CC2N(O)N=[N:19]C=2C=1.N>C(Cl)Cl.CN(C=O)C>[CH3:1][O:2][C:3]1[C:4]([CH3:12])=[C:5]([CH:9]=[CH:10][CH:11]=1)[C:6]([NH2:19])=[O:7]

参加物

6

反応物 3

HCID 222AmmoniaHCID 757711-HydroxybenzotriazoleHCID 70214833-Methoxy-2-MethylBenzoic Acid

生成物 1

HCID 160946953-Methoxy-2-methylbenzamide収率 58.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

3-Methoxy-2-methylbenzoic acid (5.0 g, 30 mmol) in CH2Cl2 (90 ml) and DMF (90 ml) was treated with HOBt (4.06 g, 30 mmol) and WSCDI (5.75 g, 30 mmol) and the resulting mixture stirred at RT for 20 min. After cooling to 0° C. ammonia (2H in EtOH, 30 ml, 60 mmol) was added and the mixture stirred for a further 2 h. The mixture was filtered, the solvent was removed from the filtrate. The crude material was taken up in CH2Cl2 and washed with water and brine and dried (Na2SO4), which gave a white solid (2.9 g) on isolation.

後処理

  1. additionwas added
  2. stirringthe mixture stirred for a further 2 h
  3. filtrationThe mixture was filtered
  4. customthe solvent was removed from the filtrate
  5. washwashed with water and brine
  6. dry with materialdried (Na2SO4), which

出典と根拠

ORDレコード
ord-4ff1234690cc47ada1da1f051ad33c7c
出典データセット
uspto-grants-2006_11
特許番号
US07138527B2

反応ノート

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