Ammonium Chloride → 3-Methoxymethyloxy-1,2-benzenedimethanol

HRID 1064834

반응식

HRID 1064834 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][CH2:9][O:10][C:11]1[CH:21]=[CH:20][CH:19]=[C:13]2[C:14]([O:16][C:17](=O)[C:12]=12)=[O:15].[Cl-].[NH4+]>O1CCCC1.CCOCC>[CH3:7][O:8][CH2:9][O:10][C:11]1[CH:21]=[CH:20][CH:19]=[C:13]([CH2:14][OH:15])[C:12]=1[CH2:17][OH:16]

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 21226445Aluminium lithium hydrideHCID 219367353-Methoxymethyloxyphthalic anhydride

생성물 1

HCID 222728523-Methoxymethyloxy-1,2-benzenedimethanol수율 60%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

After that, lithium aluminum hydride (1.14 g, 30.0 mmol) was added little by little to a solution of 3-methoxymethyloxyphthalic anhydride (3.0 g, 14.4 mmol) in anhydrous tetrahydrofuran (100 ml) under cooling with ice water and the mixture was returned to room temperature followed by stirring for 12 hours. The reaction solution was diluted with ether (300 ml) and a saturated aqueous solution (3 ml) of ammonium chloride was added thereto followed by stirring for 1 hour. The reaction solution was dried over anhydrous magnesium sulfate, filtered off through celite and the filtrate was concentrated to provide 1.71 g (yield 60%) of 3-methoxymethyloxy-1,2-benzenedimethanol as colorless oil.

후처리

  1. customwas returned to room temperature
  2. stirringby stirring for 1 hour
  3. dry with materialThe reaction solution was dried over anhydrous magnesium sulfate
  4. filtrationfiltered off through celite
  5. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-643fbb12b6c24edf9251de60c65dea63
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969711B2

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