Aluminum(III) Chloride → HCID 19047070、化合物

反応式

[H-].[Al+3].[Li+].[H-].[H-].[H-].[Al+3].[Cl-].[Cl-].[Cl-].[CH3:11][C:12]1([CH3:25])[CH2:16][C:15]2[C:17]([CH3:24])=[C:18]([CH:22]=O)[CH:19]=[C:20]([CH3:21])[C:14]=2[O:13]1>C(OCC)C>[CH3:11][C:12]1([CH3:25])[CH2:16][C:15]2[C:17]([CH3:24])=[C:18]([CH3:22])[CH:19]=[C:20]([CH3:21])[C:14]=2[O:13]1

参加物

実験手順

To a suspension of 9.75 g of lithium aluminum hydride in 200 ml of absolute diethyl ether was added 34.27 g of AlCl3 and added dropwise a mixture of 42 g of the 2,3-dihydro-2,2,4,7-tetramethylbenzofuran-5-carboxaldehyde and 27.4 g of AlCl3 in 100 ml of absolute diethyl ether. After stirring for 30 minutes, the reaction mixture was quenched with 10 ml of ethyl acetate and added with 100 ml of water and 100 ml of 2N aqueous solution of hydrochloric acid. The organic extract was dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to afford a crude product. Final purification was carried by vacuum distillation to afford 34.5 g of 2,3-dihydro-2,2,4,5,7-pentamethylbenzofuran as colorless oil.