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Sodium hydride → 1-ethyl-7-methyl-3-(4-{[tris(1-methylethyl)silyl]oxy}phenyl)-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one

HRID 82689
ノート
印刷プレビュー

反応式

HRID 82689 の反応式
[CH:1]([Si:4](Cl)([CH:8]([CH3:10])[CH3:9])[CH:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[CH2:12]([N:14]1[C:22]2[C:17](=[N:18][CH:19]=[CH:20][C:21]=2[CH3:23])[N:16]([C:24]2[CH:29]=[CH:28][C:27]([OH:30])=[CH:26][CH:25]=2)[C:15]1=[O:31])[CH3:13].[H-].[Na+].[Cl-].[Cl-].[Ca+2].C([O-])(O)=O.[Na+]>CN(C=O)C>[CH2:12]([N:14]1[C:22]2[C:17](=[N:18][CH:19]=[CH:20][C:21]=2[CH3:23])[N:16]([C:24]2[CH:29]=[CH:28][C:27]([O:30][Si:4]([CH:8]([CH3:10])[CH3:9])([CH:5]([CH3:7])[CH3:6])[CH:1]([CH3:3])[CH3:2])=[CH:26][CH:25]=2)[C:15]1=[O:31])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 24758Sodium hydrideHCID 139400Triisopropylsilyl chlorideHCID 516892Sodium BicarbonateHCID 5284359Calcium ChlorideHCID 58577432HCID 58577432、化合物

生成物 1

HCID 585775691-ethyl-7-methyl-3-(4-{[tris(1-methylethyl)silyl]oxy}phenyl)-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Triisopropylsilyl chloride (2.384 mL) was added to a solution of 1-ethyl-3-(4-hydroxyphenyl)-7-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (2 g) and NaH (0.594 g) in DMF (20 ml) at 20° C. The mixture was stirred at 20° C. under a dry atmosphere (CaCl2 tube) for 1 h. The mixture was poured into sat. NaHCO3 at 0° C. and extracted with EtOAc. The organic layer was separated, washed with water and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography (NH silica gel, eluted with 0%-25% EtOAc in hexane) to give 1-ethyl-7-methyl-3-(4-{[tris(1-methylethyl)silyl]oxy}phenyl)-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (4.0 g) as light brown crystals.

後処理

  1. extractionextracted with EtOAc
  2. customThe organic layer was separated
  3. washwashed with water and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by column chromatography (NH silica gel, eluted with 0%-25% EtOAc in hexane)

出典と根拠

ORDレコード
ord-d75d716e3a094256a25576d4fee6cefb
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08846713B2

反応ノート

読み込み中…

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