Water → beta,beta-Dimethylbenzeneethanol

HRID 704418

반응식

HRID 704418 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 219535beta,beta-Dimethylbenzeneethanol

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-74fac3b8acdc4e79b0b153b118433d96
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04987132

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