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

HRID 67149

반응식

HRID 67149 반응식
[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]

참가 물질

6

반응물 4

HCID 3051Diethyl PyrocarbonateHCID 6342Acetonitrile2회HCID 8471TriethylamineHCID 128066655-Butyryl-1,6-dimethyl-benzimidazole-2-carboxylic acid

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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°.

후처리

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

출처 및 근거

ORD 기록
ord-f9bbc6572ec74a20b197f28a15b1a56a
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344957

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