Water → 2-(Benzo[d][1,3]dioxol-5-yl)propan-2-ol

HRID 486937

反応式

HRID 486937 の反応式
[CH3:1][Li].[C:3]([C:6]1[CH:14]=[CH:13][C:9]2[O:10][CH2:11][O:12][C:8]=2[CH:7]=1)(=[O:5])[CH3:4].O>CCOCC.O1CCCC1>[O:10]1[C:9]2[CH:13]=[CH:14][C:6]([C:3]([OH:5])([CH3:1])[CH3:4])=[CH:7][C:8]=2[O:12][CH2:11]1

参加物

6

反応物 3

HCID 962WaterHCID 76622AcetopiperoneHCID 178418348HCID 178418348、化合物

生成物 1

HCID 118196322-(Benzo[d][1,3]dioxol-5-yl)propan-2-ol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

About 600 ml of a 1.5M solution of methyllithium in ether was added to 500 ml of tetrahydrofuran to obtain a mixture. A suspension of 93.45 g of 5-acetyl-1,3-benzodioxole in 900 ml of tetrahydrofuran was added to the mixture, while keeping it at -20° C. by cooling and the obtained mixture was stirred as such for one hour. Water was added to the reaction mixture and the obtained mixture was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous solution of common salt and dried over anhydrous magnesium sulfate. The resulting mixture was filtered and the filtrate was concentrated to obtain 97 g of the title compound as an oil.

後処理

  1. customto obtain a mixture
  2. additionwas added to the mixture
  3. customat -20° C.
  4. temperatureby cooling
  5. extractionthe obtained mixture was extracted with ethyl acetate
  6. washThe organic layer was washed with a saturated aqueous solution of common salt
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationThe resulting mixture was filtered
  9. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-df0f0cf173224bc2b6c7091531747244
出典データセット
uspto-grants-1994_03
特許番号
US05292901

関連ノート

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