Water → tert-Butyl 4-(hydroxymethyl)phenethylcarbamate

HRID 1668378노트

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HRID 1668378 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][CH2:10][C:11]1[CH:21]=[CH:20][C:14]([C:15](OCC)=[O:16])=[CH:13][CH:12]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[C:1]([O:5][C:6](=[O:7])[NH:8][CH2:9][CH2:10][C:11]1[CH:21]=[CH:20][C:14]([CH2:15][OH:16])=[CH:13][CH:12]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 67360059Ethyl 4-(2-(tert-butoxycarbonylamino)ethyl)benzoate

생성물 1

HCID 22337080tert-Butyl 4-(hydroxymethyl)phenethylcarbamate수율 110.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of ethyl 4-{2-[(tert-butoxycarbonyl)amino]ethyl}benzoate (4 g) in tetrahydrofuran (30 ml) was added lithium aluminum hydride (0.82 g), and the mixture was stirred at 0° C. for 30 min. Water (3.6 ml) and 1N aqueous sodium hydroxide solution (1 ml) were added to quench the reaction, and the precipitate was filtered off. The filtrate was dried over anhydrous sodium sulfate, and concentrated under reduced pressure to give the title compound (3.8 g) as a colorless oil.

후처리

  1. customto quench
  2. customthe reaction
  3. filtrationthe precipitate was filtered off
  4. dry with materialThe filtrate was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-de4567951caa4cb3ba3d6ee498c63e9d
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07989445B2

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