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

HRID 1606327ノート

反応式

HRID 1606327 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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 a brown 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.

後処理

  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 a brown residue which
  6. customcrystallised from light petroleum (b.p. 40°-60°C)

出典と根拠

ORDレコード
ord-ec7c54b1a57140d1aaa4df6e394ae49b
出典データセット
uspto-grants-1976_04
特許番号
US03952104

反応ノート

読み込み中…