N-Hydroxyacetamidine → N'-[(3,4-dimethoxy-5-nitrobenzoyl)oxy]acetamidine

HRID 725415

反応式

HRID 725415 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:13]=[C:14]([N+:18]([O-:20])=[O:19])[C:15]=1[O:16][CH3:17])[C:6](N1C=CN=C1)=[O:7].[C:21](=[N:24][OH:25])([NH2:23])[CH3:22]>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:13]=[C:14]([N+:18]([O-:20])=[O:19])[C:15]=1[O:16][CH3:17])[C:6]([O:25][N:24]=[C:21]([NH2:23])[CH3:22])=[O:7]

参加物

4

反応物 2

HCID 30926N-HydroxyacetamidineHCID 214590201-(3,4-Dimethoxy-5-nitrobenzoyl)imidazole

生成物 1

HCID 53789064N'-[(3,4-dimethoxy-5-nitrobenzoyl)oxy]acetamidine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

10.0 g of 1-(3,4-dimethoxy-5-nitrobenzoyl)imidazole in 50 ml of dimethylformamide are treated with 6.95 g of acetamidoxime, whereupon the mixture is stirred at 70° for 1 hour. After cooling, the mixture is poured into 500 ml of ice-water and stirred for 30 minutes. The separated crystals are filtered under suction and washed with water. After crystallization from ethyl acetate there is obtained N'-[(3,4-dimethoxy-5-nitrobenzoyl)oxy]acetamidine in the form of colorless crystals of m.p. 165°-166°.

後処理

  1. temperatureAfter cooling
  2. stirringstirred for 30 minutes
  3. filtrationThe separated crystals are filtered under suction
  4. washwashed with water
  5. customAfter crystallization from ethyl acetate

出典と根拠

ORDレコード
ord-77f70318cb7a43db82676fe8f25546cd
出典データセット
uspto-grants-1998_01
特許番号
US05705703

関連ノート

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