1,3-Dichloroacetone → 2-(Chloromethyl)-5,7-dimethylimidazo[1,2-a]pyrimidine
反応式
[NH2:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[Cl:10][CH2:11][C:12](=O)[CH2:13]Cl>COCCOC>[Cl:10][CH2:11][C:12]1[N:1]=[C:2]2[N:7]=[C:6]([CH3:8])[CH:5]=[C:4]([CH3:9])[N:3]2[CH:13]=1参加物
4
実験手順
A solution of 2-amino-4,6-dimethylpyrimidine (2.46 g, 20.0 mmol) and 1,3-dichloro-2-propanone (2.67 g, 21.0 mmol) in 1,2-dimethoxyethane (20 mL) was stirred at 45° C. overnight. A precipitate formed, and this was collected by filtration, and was then refluxed with ethanol (15 mL) for 2 hours. After cooling to room temperature, the product precipitated as white needles which were collected by filtration and vacuum dried to yield the title compound pure as its hydrochloride salt (883 mg, 19%). 1H NMR (500 MHz, DMSO-d6): δ7.84 (s, 1H), 6.88 (s, 1H), 4.84 (s, 2H), 2.60 (s, 3H), 2.49 (s, 3H).
後処理
- customA precipitate formed
- filtrationthis was collected by filtration
- temperaturewas then refluxed with ethanol (15 mL) for 2 hours
- customthe product precipitated as white needles which
- filtrationwere collected by filtration and vacuum
- customdried
出典と根拠
- ORDレコード
- ord-960242ca42724973ba1651581cfb3e29
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08133897B2
反応ノート
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