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

HRID 486937

반응식

HRID 486937 반응식
[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

참가 물질

6

반응물 3

HCID 962WaterHCID 76622AcetopiperoneHCID 178418348HCID 178418348, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-df0f0cf173224bc2b6c7091531747244
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292901

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