Water → 1-Indanmethanol

HRID 1253797

반응식

HRID 1253797 반응식
[CH:1]1([C:10](O)=[O:11])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[CH:1]1([CH2:10][OH:11])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH2:3][CH2:2]1

참가 물질

5

반응물 3

HCID 962WaterHCID 857281H-Indene-1-carboxylic acid, 2,3-dihydro-HCID 21226445Aluminium lithium hydride

생성물 1

HCID 2718801-Indanmethanol수율 97.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2,3-dihydro-1H-inden-1-carboxylic acid (0.50 g) in tetrahydrofuran (5.0 mL), lithium aluminum hydride (0.18 g) was added under ice-cooling and the resultant reaction mixture was stirred at room temperature for 30 minutes. To the reaction mixture, water was added under ice-cooling and the resultant reaction mixture was extracted with ethyl acetate. The organic phase was washed with a saturated saline and was dried over anhydrous sodium sulfate. From the organic phase, the solvent was distilled off under reduced pressure and the resultant residue was purified by silica gel column chromatography (eluate: n-hexane:ethyl acetate=85:15 to 75:25) to obtain the subject compound (445 mg) as a colorless oil.

후처리

  1. temperaturecooling
  2. customthe resultant reaction mixture
  3. temperaturecooling
  4. customthe resultant reaction mixture
  5. extractionwas extracted with ethyl acetate
  6. washThe organic phase was washed with a saturated saline
  7. dry with materialwas dried over anhydrous sodium sulfate
  8. distillationFrom the organic phase, the solvent was distilled off under reduced pressure
  9. customthe resultant residue was purified by silica gel column chromatography (eluate: n-hexane:ethyl acetate=85:15 to 75:25)

출처 및 근거

ORD 기록
ord-7035823aa91149e1850c5c847de48d58
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455500B2

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