Water → 2-[4-(2-Methoxycarbonyl-2-methyl-propyl)-2,6-dimethyl-phenyl]-3H-benzoimidazole-5-carboxylic acid

HRID 1360799ノート

反応式

HRID 1360799 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([C:9]([OH:11])=[O:10])[CH:5]=[CH:6][C:7]=1[NH2:8].[CH3:12][O:13][C:14](=[O:29])[C:15]([CH3:28])([CH3:27])[CH2:16][C:17]1[CH:22]=[C:21]([CH3:23])[C:20]([CH:24]=O)=[C:19]([CH3:26])[CH:18]=1.OOS([O-])=O.[K+].O>CN(C=O)C>[CH3:12][O:13][C:14]([C:15]([CH3:28])([CH3:27])[CH2:16][C:17]1[CH:18]=[C:19]([CH3:26])[C:20]([C:24]2[NH:1][C:2]3[CH:3]=[C:4]([C:9]([OH:11])=[O:10])[CH:5]=[CH:6][C:7]=3[N:8]=2)=[C:21]([CH3:23])[CH:22]=1)=[O:29]

参加物

6

反応物 4

HCID 962Water2 回HCID 692633,4-Diaminobenzoic acidHCID 23707502Potassium hydroxy sulfiteHCID 86632822Methyl 3-(4-formyl-3,5-dimethylphenyl)-2,2-dimethylpropanoate

生成物 1

HCID 669667662-[4-(2-Methoxycarbonyl-2-methyl-propyl)-2,6-dimethyl-phenyl]-3H-benzoimidazole-5-carboxylic acid

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

7.6 g of 3,4-diaminobenzenoic acid was stirred in 120 ml of DMF at room temperature. It was treated with 12.4 g of 3-(4-formyl-3,5-dimethyl-phenyl)-2,2-dimethyl-propionic acid methyl ester (the intermediate A in Example 1-62) followed by an addition of a slurry of 15 g of Oxone in 60 ml of DMF. The reaction was stirred at room temperature for 3 h and 60 mL of water was added and the pH was adjusted to 6. Additional 150 mL of water was added and the resulting precipitates were collected by filtration. The collected precipitates were washed with water and dried under vacuum to afford the title compound.

後処理

  1. customthe resulting precipitates
  2. filtrationwere collected by filtration
  3. customThe collected precipitates
  4. washwere washed with water
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-e5028e1fb88d4206ac3dc7b2f6be5c34
出典データセット
uspto-grants-2011_02
特許番号
US07879850B2

反応ノート

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