Water → beta,beta-Dimethylbenzeneethanol

HRID 704418

反応式

HRID 704418 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:13])[C:9](OC)=[O:10].O>O1CCCC1>[CH3:13][C:8]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)([CH3:7])[CH2:9][OH:10]

参加物

5

反応物 3

HCID 962WaterHCID 143498Methyl 2-methyl-2-phenylpropanoateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 219535beta,beta-Dimethylbenzeneethanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of lithium aluminum hydride (1.71 g) in tetrahydrofuran (50 ml) was dropwise added a solution of methyl 2-methyl-2-phenylpropionate (7.97 g) in tetrahydrofuran (20 ml) under ice cooling and the mixture was stirred at room temperature for 30 minutes. To the reaction solution was dropwise added water and then a saturated aqueous solution of sodium bicarbonate, and the solution was extracted with ether. The ehter layer was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resultant residue was subjected to silica gel (100 g) column chromatography. Elution with a mixture solution of hexane-ethyl acetate (2:1) gave 6.32 9 of 2-methyl-2-phenylpropanol.

後処理

  1. extractiona saturated aqueous solution of sodium bicarbonate, and the solution was extracted with ether
  2. washThe ehter layer was washed with a saturated aqueous solution of sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. washElution with a mixture solution of hexane-ethyl acetate (2:1)

出典と根拠

ORDレコード
ord-74fac3b8acdc4e79b0b153b118433d96
出典データセット
uspto-grants-1991_01
特許番号
US04987132

関連ノート

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