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Water → HCID 57517505, 화합물

HRID 2368125
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HRID 2368125 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Si:7]([O:24][CH:25]1[CH2:30][CH2:29][CH:28]([C:31](OCC)=[O:32])[CH2:27][CH2:26]1)([C:20]([CH3:23])([CH3:22])[CH3:21])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.[OH-].[Na+]>C1COCC1>[Si:7]([O:24][CH:25]1[CH2:26][CH2:27][CH:28]([CH2:31][OH:32])[CH2:29][CH2:30]1)([C:20]([CH3:23])([CH3:22])[CH3:21])([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 58018637HCID 58018637, 화합물

생성물 1

HCID 57517505HCID 57517505, 화합물수율 85.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매
2회

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온도
0 °C

실험 절차

To a suspension of lithium aluminum hydride (1.13 g) in THF (100 mL) was slowly added a solution of ethyl 4-{[tert-butyl(diphenyl)silyl]oxy}cyclohexanecarboxylate (12.2 g) in THF (100 mL) under ice-cooling. The reaction mixture was stirred at 0° C. for 1 hr, and water (1.2 mL) and 1M aqueous sodium hydroxide solution (1.2 mL) were successively added thereto. The mixture was stirred at room temperature for 30 min, and water (3.6 mL) was further added thereto. The mixture was stirred at room temperature for 1 hr, and the insoluble material was filtered off through celite under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (9.38 g).

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature for 30 min
  3. stirringThe mixture was stirred at room temperature for 1 hr
  4. filtrationthe insoluble material was filtered off through celite under reduced pressure
  5. customThe obtained residue was purified by silica gel chromatography (hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-ec22dd554b694e72af74d513ea672ab1
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08703758B2

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