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Water → HCID 178426342, 화합물

HRID 1179699
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HRID 1179699 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C[O:8][C:9]1[N:14]=[CH:13][C:12]([N:15]2[C:20](=O)[CH2:19][C:18]([CH3:23])([CH3:22])[CH2:17][C:16]2=O)=[CH:11][CH:10]=1.O.[OH-].[Na+]>C(OCC)C>[CH3:22][C:18]1([CH3:23])[CH2:17][CH2:16][N:15]([C:12]2[CH:13]=[N:14][C:9]([OH:8])=[CH:10][CH:11]=2)[CH2:20][CH2:19]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 22047806HCID 22047806, 화합물

생성물 1

HCID 178426342HCID 178426342, 화합물수율 62.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Under a nitrogen atmosphere lithium aluminium hydride (1.90 g, 50.0 mmol) was added portionwise to a-stirred suspension of 6′-methoxy-4,4-dimethyl-4,5-dihydro-3H-[1,3′]bipyridinyl-2,6-dione (2.85 g, 10.0 mmol) in dry diethyl ether (100 mL). After stirring for 3 hours at room temperature, water (1.90 mL), 15% aqueous sodium hydroxide (1.90 mL) and water (5.70 mL) were added respectively. After stirring for 1 hour at room temperature the salts were removed by filtration and washed three times with diethyl ether. The solvent was evaporated in vacuo and the residue was purified by flash column chromatography (SiO2, dichloromethane followed by ethyl acetate/heptane 25/75) yielding the title compound (1.28 g, 58% yield) as a yellow oil.

후처리

  1. stirringAfter stirring for 1 hour at room temperature the salts
  2. customwere removed by filtration
  3. washwashed three times with diethyl ether
  4. customThe solvent was evaporated in vacuo
  5. customthe residue was purified by flash column chromatography (SiO2, dichloromethane followed by ethyl acetate/heptane 25/75)

출처 및 근거

ORD 기록
ord-2c18517834fd4f269f6a83ce01db608e
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07279470B2

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