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Hydrochloric Acid → HCID 17816488, 화합물

HRID 2249696
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HRID 2249696 반응식
[NH2:1][C:2]1[C:10]([Br:11])=[C:9]([C:12]([O:14][CH3:15])=[O:13])[C:8]([Br:16])=[CH:7][C:3]=1C(O)=O.C([N:19]([CH2:22]C)CC)C.C1(P(N=[N+]=[N-])(C2C=CC=CC=2)=[O:31])C=CC=CC=1.Cl>O1CCOCC1.O.C(OCC)(=O)C>[Br:11][C:10]1[C:2]2[NH:1][C:22](=[O:31])[NH:19][C:3]=2[CH:7]=[C:8]([Br:16])[C:9]=1[C:12]([O:14][CH3:15])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 199401P,P-Diphenylphosphinic azideHCID 17816503HCID 17816503, 화합물

생성물 1

HCID 17816488HCID 17816488, 화합물

시약·촉매·용매 3

HCID 962Water용매
HCID 8857
Ethyl Acetate
용매
HCID 312751,4-Dioxane용매

실험 절차

In 10 ml of dioxane is added 1.00 g of 2-amino-3,5-dibromo-4-(methoxycarbonyl)benzoic acid, to which are successively added 0.6 ml of triethylamine and 0.9 ml of diphenyl phosphoryl azide. The mixture thus obtained is heated under reflux for 1.5 hours. Ethyl acetate and water are added to the reaction mixture, pH is adjusted to 6 with 6 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, 0.96 g of methyl 4,6-dibromo-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate is obtained as a light brown-colored solid product.

후처리

  1. customThe mixture thus obtained
  2. temperatureis heated
  3. temperatureunder reflux for 1.5 hours
  4. customthe organic layer is separated
  5. customThe organic layer thus obtained
  6. washis washed with water and saturated aqueous solution of sodium chloride successively
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-659a4e6a416b43c181db6a23ef538a41
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07314888B1

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