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Water → HCID 15007049, 화합물

HRID 1613942
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HRID 1613942 반응식
[CH3:1][C:2]1[C:11]([CH3:12])=[C:10]([O:13][C:14](=[O:16])[CH3:15])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[Se](=O)=[O:18].O>O1CCOCC1>[CH:1]([C:2]1[C:11]([CH3:12])=[C:10]([O:13][C:14](=[O:16])[CH3:15])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1)=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24007Selenium DioxideHCID 15007064HCID 15007064, 화합물

생성물 1

HCID 15007049HCID 15007049, 화합물수율 52.3%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 4.30 g (20.0 mmols) of 2,3-dimethyl-4-acetoxyquinoline, 2.44 g (22.0 mmols) of selenium dioxide, 8 ml of water and 80 ml 1,4-dioxane was refluxed for 3 hours. The solvent was distilled off under reduced pressure, after which 100 ml of chloroform was added, followed by washing with a saturated sodium hydrogencarbonate aqueous solution and then with water, and drying with sodium sulfate. The solvent was distilled off under reduced pressure and the resultant crude product was purified by silica gel column chromatography (Wako Gel C-200) (solvent: n-hexane : ethyl acetate=10:1) to obtain 2.40 g (yield 52%) of 2-formyl-3-methyl-4-acetoxyquinoline.

후처리

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionafter which 100 ml of chloroform was added
  3. washby washing with a saturated sodium hydrogencarbonate aqueous solution
  4. dry with materialwith water, and drying with sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customthe resultant crude product was purified by silica gel column chromatography (Wako Gel C-200) (solvent: n-hexane : ethyl acetate=10:1)

출처 및 근거

ORD 기록
ord-2ed5f8f466d84e64a8a1cd8bdbc0b777
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05194617

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