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Sodium sulfate decahydrate → 2-[3,5-Bis(methoxymethoxy)phenyl]ethanol

HRID 499861
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HRID 499861 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][CH2:9][O:10][C:11]1[CH:12]=[C:13]([CH2:21][C:22](OC)=[O:23])[CH:14]=[C:15]([O:17][CH2:18][O:19][CH3:20])[CH:16]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:7][O:8][CH2:9][O:10][C:11]1[CH:12]=[C:13]([CH2:21][CH2:22][OH:23])[CH:14]=[C:15]([O:17][CH2:18][O:19][CH3:20])[CH:16]=1
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참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23116398Methyl 3,5-bis(methoxymethoxy)phenylacetate

생성물 1

HCID 231163592-[3,5-Bis(methoxymethoxy)phenyl]ethanol수율 98%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
4 °C

실험 절차

A solution of lithium aluminum hydride (1.0 g, 26 mmol) in tetrahydrofuran (50 mL) was cooled to 4° C., and a solution of methyl 3,5-bis(methoxymethoxy)phenylacetate (5.3 g, 20 mmol) obtained in Example 1, Step 1 in tetrahydrofuran (50 mL) was added dropwise thereto, followed by stirring at 4° C. for 30 minutes. To the reaction mixture was added anhydrous sodium sulfate decahydrate to stop the reaction, and the mixture was stirred at room temperature for 12 hours. The resulting suspension was filtered under reduced pressure, and the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/9-1/1) to obtain 2-[3,5-bis(methoxymethoxy)phenyl]ethanol (4.6 g, 98%).

후처리

  1. customthe reaction
  2. stirringthe mixture was stirred at room temperature for 12 hours
  3. filtrationThe resulting suspension was filtered under reduced pressure
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane=1/9-1/1)

출처 및 근거

ORD 기록
ord-6d225c30d1ae44e39d28c5e58dbe5ee0
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07767693B2

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