Diethyl Pyrocarbonate → Ethyl 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylate

HRID 67149

反応式

HRID 67149 の反応式
[C:1]([C:6]1[C:18]([CH3:19])=[CH:17][C:9]2[N:10]([CH3:16])[C:11]([C:13]([OH:15])=[O:14])=[N:12][C:8]=2[CH:7]=1)(=[O:5])[CH2:2][CH2:3][CH3:4].[C:20](#N)[CH3:21].C(N(CC)CC)C.C(OC(OCC)=O)(=O)OCC>C(OCC)(=O)C>[C:1]([C:6]1[C:18]([CH3:19])=[CH:17][C:9]2[N:10]([CH3:16])[C:11]([C:13]([O:15][CH2:20][CH3:21])=[O:14])=[N:12][C:8]=2[CH:7]=1)(=[O:5])[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 3051Diethyl PyrocarbonateHCID 6342Acetonitrile2 回HCID 8471TriethylamineHCID 128066655-Butyryl-1,6-dimethyl-benzimidazole-2-carboxylic acid

生成物 1

HCID 12806645Ethyl 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylate

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

6.0 g of 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylic acid are introduced, in the course of 15 minutes, into a mixture of 150 ml of acetonitrile, 15 ml of triethylamine and 18.5 g of diethyl pyrocarbonate, while stirring at room temperature. The mixture is left to stand overnight, the acetonitrile is stripped off under reduced pressure, the residue is taken up in ethyl acetate and the resulting solution is washed with water, dried over sodium sulphate and evaporated to dryness. Ethyl 5-butyryl-1,6-dimethyl-benzimidazole-2-carboxylate, which is initially obtained as an oil but soon crystallises, is filtered off. When recrystallised from ethyl acetate/cyclohexane, it melts at 106°-108°.

後処理

  1. waitThe mixture is left
  2. washthe resulting solution is washed with water
  3. dry with materialdried over sodium sulphate
  4. customevaporated to dryness

出典と根拠

ORDレコード
ord-f9bbc6572ec74a20b197f28a15b1a56a
出典データセット
uspto-grants-1982_08
特許番号
US04344957

関連ノート

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