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Water → HCID 178426342、化合物

HRID 1179699
ノート
印刷プレビュー

反応式

HRID 1179699 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 22047806HCID 22047806、化合物

生成物 1

HCID 178426342HCID 178426342、化合物収率 62.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2c18517834fd4f269f6a83ce01db608e
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07279470B2

反応ノート

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