Sodium hydride → HCID 22058664、化合物
反応式
[H-].[Na+].[Br:3][C:4]1[N:5]=[C:6]([CH3:10])[NH:7][C:8]=1[Br:9].[CH3:11][Si:12]([CH3:19])([CH3:18])[CH2:13][CH2:14][O:15][CH2:16]Cl>>[Br:3][C:4]1[N:5]=[C:6]([CH3:10])[N:7]([CH2:16][O:15][CH2:14][CH2:13][Si:12]([CH3:19])([CH3:18])[CH3:11])[C:8]=1[Br:9]参加物
実験手順
A 901 mg portion of 60% sodium hydride was added little by little to ice-cold N,N-dimethylformamide (50 ml) containing 4.91 g of 4,5-dibromo-2-methylimidazole. The reaction mixture was stirred at room temperature for 1 hour. 2-(Trimethysilyl)ethoxymethyl chloride (3.75 g) was added dropwise to the mixture on ice, and the mixture was stirred at room temperature overnight. The solvent was evaporated under reduced pressure, ethyl acetate was added to the resulting residue, and the mixture was washed subsequently with a saturated sodium hydrogen carbonate aqueous solution and a sodium chloride aqueous solution. The organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was purified by silica-gel column chromatography (eluent, hexane:ethyl acetate=3:1) to obtain 7.6 g of colorless oily material of 4,5-dibromo-2-methyl-1-(2-(trimethylsilyl)ethoxymethyl)imidazole.
後処理
- stirringthe mixture was stirred at room temperature overnight
- customThe solvent was evaporated under reduced pressure, ethyl acetate
- additionwas added to the resulting residue
- washthe mixture was washed subsequently with a saturated sodium hydrogen carbonate aqueous solution
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- customthe solvent was evaporated under reduced pressure
- customThe resulting residue was purified by silica-gel column chromatography (eluent, hexane:ethyl acetate=3:1)
出典と根拠
- ORDレコード
- ord-8791a4efc0d6403684741ac0219ff584
- 出典データセット
- uspto-grants-2001_06
- 特許番号
- US06242474B1
反応ノート
読み込み中…