Acetone → HCID 54382404、化合物

HRID 1870628ノート

反応式

HRID 1870628 の反応式
[CH3:1][C:2]1([CH3:16])[CH2:10][C:9]2[C:4](=[C:5]([CH3:15])[C:6]([CH3:14])=[C:7]([CH:12]=O)[C:8]=2[CH3:11])[CH2:3]1.O.[OH-].[Na+].Cl.[CH3:21][C:22]([CH3:24])=[O:23]>>[CH3:1][C:2]1([CH3:16])[CH2:3][C:4]2[C:9](=[C:8]([CH3:11])[C:7]([CH3:12])=[C:6]([CH:14]=[CH:21][C:22](=[O:23])[CH3:24])[C:5]=2[CH3:15])[CH2:10]1

参加物

6

反応物 5

HCID 180AcetoneHCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium HydroxideHCID 137335152,2,4,6,7-Pentamethyl-2,3-dihydro-1H-indene-5-carbaldehyde

生成物 1

HCID 54382404HCID 54382404、化合物収率 79%

実験手順

To a solution of 26.8 g of the 2,2,4,6,7-pentamethylindan-5-carboxaldehyde in 93 ml of absolute acetone was added 46 ml of water and 50 g of 2% NaOH. After refluxing for 20 hours, the solution was acidified with 2N HCl and extracted with diethyl ether. The organic layer was dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by silica-gel column chromatography to afford 25.36 g of the title compound as yellow solid.

後処理

  1. temperatureAfter refluxing for 20 hours
  2. extractionextracted with diethyl ether
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residue was purified by silica-gel column chromatography

出典と根拠

ORDレコード
ord-75c1ed6ca6f34057b0875df4a9532510
出典データセット
uspto-grants-2000_08
特許番号
US06096930

反応ノート

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