Water → 2-(3,4-dihydro-2H-1-benzopyran-3-yl)ethan-1-ol

HRID 1196011노트

반응식

HRID 1196011 반응식
C[O:2][C:3]([CH2:5][CH:6]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[O:8][CH2:7]1)=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1.C(OCC)C>[OH:2][CH2:3][CH2:5][CH:6]1[CH2:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[O:8][CH2:7]1

참가 물질

7

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 148384133-MethoxycarbonylmethylchromanHCID 21226445Aluminium lithium hydride

생성물 1

HCID 148384142-(3,4-dihydro-2H-1-benzopyran-3-yl)ethan-1-ol수율 100%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

At room temperature and while stirring, a solution of 7.22 g (35 mmol) of 3-methoxycarbonylmethylchroman in 50 ml of absolute tetrahydrofuran is added dropwise within a period of 30 minutes to a suspension of 1.33 g (35 mmol) of lithium aluminium hydride in 50 ml of absolute diethyl ether. Stirring is continued at room temperature for a further 16 hours and then the whole is carefully decomposed with 1.33 ml of water, 1.33 ml of sodium hydroxide solution (15% strength) and 4.0 ml of water. The precipitate formed is filtered off with suction and the filtrate is concentrated by evaporation in vacuo. The oily residue is dissolved in diethyl ether. The solution is washed with water, dried over sodium sulphate and concentrated by evaporation in vacuo. 6.23 g (100%) of 3-(2-hydroxyethyl)chroman are obtained in the form of a yellow oil.

후처리

  1. stirringStirring
  2. customThe precipitate formed
  3. filtrationis filtered off with suction
  4. concentrationthe filtrate is concentrated by evaporation in vacuo
  5. dissolutionThe oily residue is dissolved in diethyl ether
  6. washThe solution is washed with water
  7. dry with materialdried over sodium sulphate
  8. concentrationconcentrated by evaporation in vacuo

출처 및 근거

ORD 기록
ord-553feeef9a354977acd39ed6b7be6582
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112855

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