反応式
[H-].[Na+].[CH3:3][CH:4]([CH3:8])[CH:5]([OH:7])[CH3:6].Cl[C:10]1[CH:15]=[C:14](Cl)[N:13]=[CH:12][N:11]=1.[CH2:17]([OH:22])[C:18]#[C:19][CH2:20][CH3:21].[Cl-].[NH4+]>O1CCCC1>[CH3:6][CH:5]([O:7][C:10]1[CH:15]=[C:14]([O:22][CH2:17][C:18]#[C:19][CH2:20][CH3:21])[N:13]=[CH:12][N:11]=1)[CH:4]([CH3:8])[CH3:3]参加物
実験手順
In 4 ml of tetrahydrofuran was suspended 0.13 g of sodium hydride (60% in oil), to which 0.5 ml of a solution containing 0.24 g of 3-methyl-2-butanol was added dropwise at 0° C., followed by stirring for 10 minutes. To this was added dropwise 0.5 ml of a solution containing 0.40 g of 4,6-dichloropyrimidine in tetrahydrofuran, followed by stirring at 0° C. for 3 hours. To this was added dropwise 0.5 ml of a solution containing 0.29 g of 2-pentyn-1-ol in tetrahydrofuran and further added 0.15 g of sodium hydride (60% in oil), followed by stirring at room temperature for 4 hours. The reaction mixture was then poured into a saturated aqueous ammonium chloride solution, which was extracted three times with t-butyl methyl ether. The combined organic layers were washed with a saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and then concentrated. The residue was subjected to silica gel column chromatography to give 0.44 g of 4-(1,2-dimethylpropyloxy)-6-(2-pentynyloxy)pyrimidine (the present compound (22)).
後処理
- additionwas added dropwise at 0° C.
- stirringby stirring at 0° C. for 3 hours
- stirringby stirring at room temperature for 4 hours
- extractionwas extracted three times with t-butyl methyl ether
- washThe combined organic layers were washed with a saturated aqueous sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-8cf4cc48cefe424398aa114ac6a0a4dd
- 出典データセット
- uspto-grants-2007_05
- 特許番号
- US07223769B2
関連ノート
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