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Water → 1-(6-Methyl-1,3-benzodioxol-5-yl)ethanol

HRID 486890
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HRID 486890 반응식
[CH3:1][Li].[CH3:3][C:4]1[C:9]([CH:10]=[O:11])=[CH:8][C:7]2[O:12][CH2:13][O:14][C:6]=2[CH:5]=1.O>C(OCC)C.O1CCCC1>[CH3:3][C:4]1[C:9]([CH:10]([OH:11])[CH3:1])=[CH:8][C:7]2[O:12][CH2:13][O:14][C:6]=2[CH:5]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 31462426-Methyl-2H-1,3-benzodioxole-5-carbaldehydeHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 145148961-(6-Methyl-1,3-benzodioxol-5-yl)ethanol

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

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온도
-40 °C

실험 절차

32 ml of a 1.4M solution of methyllithium in diethyl ether was dissolved in 50 ml of anhydrous tetrahydrofuran and the solution was cooled at -40° C. in a nitrogen atmosphere. 5.0 g of solid (6-methyl-1,3-benzodioxol-5-yl) carboxaldehyde was added to the solution and the temperature was elevated to room temperature gradually over 1 h. Water was added to the reaction mixture. After extraction with ether, the organic layer was washed with an aqueous common salt solution. After drying over magnesium sulfate, the solvent was distilled off to obtain a white solid, which was recrystallized from diisopropyl ether/n-hexane to obtain 2.8 g of the intended compound in the form of white crystals.

후처리

  1. extractionAfter extraction with ether
  2. washthe organic layer was washed with an aqueous common salt solution
  3. dry with materialAfter drying over magnesium sulfate
  4. distillationthe solvent was distilled off
  5. customto obtain a white solid, which
  6. customwas recrystallized from diisopropyl ether/n-hexane

출처 및 근거

ORD 기록
ord-1ec77b5659234381a93e3e48556e8f1c
출처 데이터셋
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05292901

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