Water → 2-[Bis(4-methoxymethoxyphenyl)methyl]benzyl alcohol

HRID 1196168노트

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HRID 1196168 반응식
[CH3:1][O:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]([C:24]2[CH:29]=[CH:28][C:27]([O:30][CH2:31][O:32][CH3:33])=[CH:26][CH:25]=2)[C:12]2[CH:23]=[CH:22][CH:21]=[CH:20][C:13]=2[C:14](OCOC)=[O:15])=[CH:7][CH:6]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[CH3:33][O:32][CH2:31][O:30][C:27]1[CH:26]=[CH:25][C:24]([CH:11]([C:8]2[CH:7]=[CH:6][C:5]([O:4][CH2:3][O:2][CH3:1])=[CH:10][CH:9]=2)[C:12]2[CH:23]=[CH:22][CH:21]=[CH:20][C:13]=2[CH2:14][OH:15])=[CH:29][CH:28]=1

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 19938166Methoxymethyl 2-[bis(4-methoxymethoxyphenyl)methyl]benzoateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 539143042-[Bis(4-methoxymethoxyphenyl)methyl]benzyl alcohol수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

In 500 ml of tetrahydrofuran was dissolved 74 g of methoxymethyl 2-[bis(4-methoxymethoxyphenyl)methyl]benzoate obtained by Reference Example 3. The solution was ice-cooled, 10 g of lithium aluminum hydride was added thereto, and the mixture was stirred for 10 minutes. The reaction mixture was stirred for additional 30 minutes at room temperature, and ice cooled, and then 10 ml of water, 10 ml of aqueous 15% sodium hydroxide and 30 ml of water were added thereto in order. The mixture was filtered by use of a filter aid and then concentrated under reduced pressure to afford 53.54 g of the desired compound as an oily matter.

후처리

  1. customobtained by Reference Example 3
  2. temperaturecooled
  3. stirringThe reaction mixture was stirred for additional 30 minutes at room temperature
  4. temperatureice cooled
  5. filtrationThe mixture was filtered by use of a filter aid
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-816e962ea96e4a009d0b07174d96a87a
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112867

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