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

HRID 1195300
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HRID 1195300 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
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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 1.4 M solution of methyllithium in diethyl ether was dissolved in 50 ml of anhydrous tetrahydrofuran. The obtained solution was cooled to -40° C. in a nitrogen atmosphere, followed by the addition of 5.0 g of solid (6-methyl-1,3-benzodioxol-5-yl)carboxaldehyde. The mixture was heated to a room temperature over a period of one hour, followed by the addition of water. The obtained mixture was extracted with ether and the obtained organic layer was washed with an aqueous solution of common salt, dried over magnesium sulfate and distilled to remove the solvent. The obtained white solid was recrystallized from diisopropyl ether/n-hexane to obtain 2.8 g of the title compound as a colorless crystal.

후처리

  1. temperatureThe mixture was heated to a room temperature over a period of one hour
  2. extractionThe obtained mixture was extracted with ether
  3. washthe obtained organic layer was washed with an aqueous solution of common salt
  4. dry with materialdried over magnesium sulfate
  5. distillationdistilled
  6. customto remove the solvent
  7. customThe obtained white solid was recrystallized from diisopropyl ether/n-hexane

출처 및 근거

ORD 기록
ord-0e904d4f277f4e3b923ad74d8b62d5b6
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05110956

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