Selenium Dioxide → 6,8-di-t-butyl-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester

HRID 973272노트

반응식

HRID 973272 반응식
[C:1]([C:5]1[CH:6]=[C:7]([C:21]([CH3:24])([CH3:23])[CH3:22])[C:8]2[O:13][CH:12]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[CH2:11][C:10](=[O:19])[C:9]=2[CH:20]=1)([CH3:4])([CH3:3])[CH3:2].[Se](=O)=O>CCOCC>[C:1]([C:5]1[CH:6]=[C:7]([C:21]([CH3:22])([CH3:24])[CH3:23])[C:8]2[O:13][C:12]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:11][C:10](=[O:19])[C:9]=2[CH:20]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

4

반응물 2

HCID 24007Selenium DioxideHCID 867332766,8-di-t-butyl-2,3-dihydro-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester

생성물 1

HCID 538439426,8-di-t-butyl-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 3.32 parts of 6,8-di-t-butyl-2,3-dihydro-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester and 3.33 parts of selenium dioxide was refluxed in 35 parts of xlene for eight hours. The reaction mixture was cooled, ether was added and the insoluble inorganic products were removed by filtration. Evaporation of the volatile components of the filtrate gave abrown residue which crystallised from light petroleum (b.p. 40°-60° C) to give 1.54 parts of 6,8-di-t-butyl-4-oxo-4H-1-benzopyran-2-carboxylic acid, ethyl ester, m.p. 130°-131.5° C.

후처리

  1. temperaturewas refluxed in 35 parts of xlene for eight hours
  2. temperatureThe reaction mixture was cooled
  3. customthe insoluble inorganic products were removed by filtration
  4. customEvaporation of the volatile components of the filtrate
  5. customgave abrown residue which
  6. customcrystallised from light petroleum (b.p. 40°-60° C)

출처 및 근거

ORD 기록
ord-8d18eee452f04faf9e16c5d59d3d5b70
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04055654

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