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

HRID 486939
ノート
印刷プレビュー

反応式

HRID 486939 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 962WaterHCID 31462426-Methyl-2H-1,3-benzodioxole-5-carbaldehydeHCID 178418348HCID 178418348、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-40 °C

実験手順

32 ml of a 1.4M 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.

後処理

  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

出典と根拠

ORDレコード
ord-23d7532876f345229ad035a20b9f9565
出典データセット
uspto-grants-1994_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05292901

反応ノート

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