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Hydrochloric Acid → HCID 17816478, 화합물

HRID 2249697
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HRID 2249697 반응식
[Br:1][C:2]1[C:10]2[NH:9][C:8](=[O:11])[NH:7][C:6]=2[CH:5]=[C:4]([Br:12])[C:3]=1[C:13]([O:15][CH3:16])=[O:14].[H-].[Na+].[CH2:19](Br)[CH2:20][CH:21]([CH3:23])[CH3:22].Cl>CN(C)C=O.O.C(OCC)(=O)C>[Br:1][C:2]1[C:10]2[N:9]([CH2:19][CH2:20][CH:21]([CH3:23])[CH3:22])[C:8](=[O:11])[N:7]([CH2:10][CH2:2][CH:3]([CH3:13])[CH3:4])[C:6]=2[CH:5]=[C:4]([Br:12])[C:3]=1[C:13]([O:15][CH3:16])=[O:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 78911-Bromo-3-methylbutaneHCID 24758Sodium hydrideHCID 17816488HCID 17816488, 화합물

생성물 1

HCID 17816478HCID 17816478, 화합물

시약·촉매·용매 3

HCID 962Water용매
HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

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온도
55 °C

실험 절차

In 10 ml of N,N-dimethylformamide are suspended 0.95 g of methyl 4,6-dibromo-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate, 0.24 g of 60% sodium hydride and 0.7 ml of isopentyl bromide. The suspension is stirred at 50-60° C. for 3 hours. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 2 with 2 mol/L hydrochloric acid, and the organic layer is separated. The organic layer thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and then the solvent is distilled off under reduced pressure. Thus, 0.71 g of methyl 4,6-dibromo-1,3-diisopentyl-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate is obtained as a light brown-colored solid product.

후처리

  1. customthe organic layer is separated
  2. customThe organic layer thus obtained
  3. washis washed with water and saturated aqueous solution of sodium chloride successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-8be4fc6a151945349a1ce116a9ce0165
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314888B1

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