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Methanol → 4H-Pyran-3-carboxylic acid, 2,6-dimethyl-4-oxo-, methyl ester

HRID 2072294
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반응식

HRID 2072294 반응식
[C:1]([C:4]1[C:9](=[O:10])[CH:8]=[C:7]([CH3:11])[O:6][C:5]=1[CH3:12])([OH:3])=[O:2].[C:13](Cl)(=O)C.CO.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[C:1]([C:4]1[C:9](=[O:10])[CH:8]=[C:7]([CH3:11])[O:6][C:5]=1[CH3:12])([O:3][CH3:13])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 6367Acetyl chlorideHCID 10340Sodium CarbonateHCID 2011052,6-Dimethyl-4-oxo-4H-pyran-3-carboxylic acid

생성물 1

HCID 122813714H-Pyran-3-carboxylic acid, 2,6-dimethyl-4-oxo-, methyl ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

42 g of 3-carboxy-2,6-dimethylpyr-4-one is dissolved in 250 ml of methylene chloride. In a second flask, 20 ml of acetyl chloride is cautiously added to 400 ml of methanol. The two solutions are mixed and refluxed for five hours. Solid sodium carbonate is added and the solvent removed after a water wash. The residue is distilled (115°-125° at 0.1 mm) to give 40 g of 3-carbomethoxy-2,6-dimethylpyr-4-one as a waxy solid.

후처리

  1. additionThe two solutions are mixed
  2. temperaturerefluxed for five hours
  3. customthe solvent removed after a water
  4. washwash
  5. distillationThe residue is distilled (115°-125° at 0.1 mm)

출처 및 근거

ORD 기록
ord-5d18beedd07a42abb6f9921a2a369e22
출처 데이터셋
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04051142

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