反応式
[CH3:1][C:2]([Si:5]([CH3:21])([CH3:20])[O:6][CH2:7][C:8]1[CH:13]=[C:12]([O:14]C)[N:11]=[C:10]([CH2:16][CH2:17][CH2:18]O)[CH:9]=1)([CH3:4])[CH3:3].N1C=CC=CC=1.FC(F)(F)S(OS(C(F)(F)F)(=O)=O)(=O)=O.O>ClCCl.[I-].C([N+](CCCC)(CCCC)CCCC)CCC>[CH3:1][C:2]([Si:5]([CH3:21])([CH3:20])[O:6][CH2:7][C:8]1[CH:9]=[C:10]2[N:11]([CH2:18][CH2:17][CH2:16]2)[C:12](=[O:14])[CH:13]=1)([CH3:4])[CH3:3]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
A solution of 3-[4-({[(1,1-dimethylethyl)(dimethyl)silyl]oxy}methyl)-6-(methyloxy)-2-pyridinyl]-1-propanol (5.16 g, 16.59 mmol) in dichloromethane (250 ml) was treated with pyridine (2.94 ml, 36.47 mmol) and trifluoromethanesulfonic anhydride (3.1 ml, 19.88 mmol) and stirred at room temperature for 10 min before being treated with tetrabutylammonium iodide (30.61 g, 82.95 mmol) and stirred at room temperature for a further 4 h. Water was then added and the mixture was extracted three times with diethyl ether and the combined organic extracts washed again with water. The organic extracts were dried with magnesium sulphate and evaporated. The residue was chromatographed on silica eluting with 0-10% methanol in dichloromethane to give the desired product (3.93 g, 14.09 mmol)
後処理
- stirringstirred at room temperature for a further 4 h
- extractionthe mixture was extracted three times with diethyl ether
- washthe combined organic extracts washed again with water
- dry with materialThe organic extracts were dried with magnesium sulphate
- customevaporated
- customThe residue was chromatographed on silica eluting with 0-10% methanol in dichloromethane
出典と根拠
- ORDレコード
- ord-3cf1578bc419485980131438e0738c79
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07732461B2
関連ノート
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