Ethyl ketone → ethyl 5-(4,5-dimethoxy-2-nitrobenzoyl)-2-(3-methoxypentan-3-yl)-2H-1,2,3-triazole-4-carboxylate

HRID 841971ノート

反応式

HRID 841971 の反応式
O.[C:2]1(C)[CH:7]=[CH:6]C(S(O)(=O)=O)=[CH:4][CH:3]=1.CC[C:15](=[O:18])CC.C(OC)(OC)OC.[CH3:26][O:27][C:28]1[C:45]([O:46][CH3:47])=[CH:44][C:31]([C:32]([C:34]2[NH:38][N:37]=[N:36][C:35]=2[C:39]([O:41][CH2:42][CH3:43])=[O:40])=[O:33])=[C:30]([N+:48]([O-:50])=[O:49])[CH:29]=1>C(Cl)Cl.C(N(CC)CC)C>[CH3:26][O:27][C:28]1[C:45]([O:46][CH3:47])=[CH:44][C:31]([C:32]([C:34]2[C:35]([C:39]([O:41][CH2:42][CH3:43])=[O:40])=[N:36][N:37]([C:2]([O:18][CH3:15])([CH2:7][CH3:6])[CH2:3][CH3:4])[N:38]=2)=[O:33])=[C:30]([N+:48]([O-:50])=[O:49])[CH:29]=1

参加物

7

実験手順

p-Toluenesulfonic acid monohydrate (20 mg) was added to a solution of 3-pentanone (3.1 ml) and trimethyl orthoformate (3.3 ml) in methylene chloride (10 ml). The mixture was heated for one hr with stirring. This solution (4 ml) was added to a solution of ethyl 5-(4,5-dimethoxy-2-nitrobenzoyl)-1H-1,2,3-triazole-4-carboxylate (Synthesis Example 2) (140 mg) in methylene chloride (2 ml). The mixture was stirred at room temperature for one hr, and triethylamine (0.05 ml) was then added thereto. The mixture was post-treated by a conventional method and subjected to separation and purification to give ethyl 5-(4,5-dimethoxy-2-nitrobenzoyl)-2-(3-methoxypentan-3-yl)-2H-1,2,3-triazole-4-carboxylate (140 mg, 78%) as a yellow powder.

後処理

  1. temperatureThe mixture was heated for one hr
  2. stirringThe mixture was stirred at room temperature for one hr
  3. additionThe mixture was post-treated by a conventional method
  4. customsubjected to separation and purification

出典と根拠

ORDレコード
ord-a1da1e59376f4493b1f97a6190d14fe6
出典データセット
uspto-grants-2002_04
特許番号
US06372735B1

反応ノート

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