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Water → Ethyl (pyridin-4-yl)glyoxylate Hydrate

HRID 352822
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HRID 352822 반응식
Cl.Br[CH:3]([C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1)[C:4]([O:6][CH2:7][CH3:8])=[O:5].[N-]=[N+]=[N-].[Na+].[OH2:19]>CN(C)C=O>[OH2:5].[N:12]1[CH:13]=[CH:14][C:9]([C:3](=[O:19])[C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH:10][CH:11]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 33557Sodium AzideHCID 86592085Ethyl 2-bromo-2-(pyridin-4-yl)acetate hydrochloride

생성물 1

HCID 86592084Ethyl (pyridin-4-yl)glyoxylate Hydrate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Ethyl bromo(pyridin-4-yl)acetate hydrochloride (2.05 g) was dissolved in N,N-dimethylformamide (10 ml) at room temperature, followed by the addition of sodium azide (1.43 g). The resulting mixture was stirred for 30 minutes. After the addition of water and stirring, the insoluble matter was filtered off and the filtrate was concentrated. The residue was extracted with diethyl ether and saturated aqueous NaCl solution. The organic layer thus obtained was dried over anhydrous magnesium sulfate. The filtrate was concentrated and the residue was crystallized from methylene chloride, whereby the title compound (yellow powder, 300 mg) was obtained.

후처리

  1. stirringstirring
  2. filtrationthe insoluble matter was filtered off
  3. concentrationthe filtrate was concentrated
  4. extractionThe residue was extracted with diethyl ether and saturated aqueous NaCl solution
  5. customThe organic layer thus obtained
  6. dry with materialwas dried over anhydrous magnesium sulfate
  7. concentrationThe filtrate was concentrated
  8. customthe residue was crystallized from methylene chloride, whereby the title compound (yellow powder, 300 mg)
  9. customwas obtained

출처 및 근거

ORD 기록
ord-af0f406eab674e9abf6da64aae12a3bd
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06747023B1

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