Methyl Ethyl Ketone → HCID 21409920、化合物
反応式
[CH3:1][NH:2][C:3]([CH3:7])([CH3:6])[C:4]#[N:5].[CH2:8](Br)[CH:9]=[CH2:10].C(=O)([O-])[O-].[Na+].[Na+].C(C(C)=O)C>CCOCC.[I-].[Na+]>[CH2:10]([CH2:1][NH:2][C:3]([CH3:7])([CH3:6])[C:4]#[N:5])[CH:9]=[CH2:8]参加物
7
実験手順
A mixture of 2-methylamino-2-methylpropionitrile (14.7 g., 0.15 mole) allyl bromide (18.0 g., 0.15 mole), sodium carbonate (15.9 g., 0.15 mole), sodium iodide (0.2 g., 0.001 mole) and methyl ethyl ketone (200 ml.) was heated under reflux for 40 hrs. The sodium carbonate was filtered off and the solvent was removed from the filtrate in vacuo to give a yellow oil, T.L.C. (Silica, ether), three components RF 0.8, 0.4 and 0.0. The oil was passed through a column of silica 40 × 3.5 cm. using ether as an eluent to give 2-allylmethylamino-2-methylpropionitrile (10.0 g., 48%).
後処理
- temperaturewas heated
- temperatureunder reflux for 40 hrs
- filtrationThe sodium carbonate was filtered off
- customthe solvent was removed from the filtrate in vacuo
- customto give a yellow oil, T.L.C
出典と根拠
- ORDレコード
- ord-15a041ce1daf4d72a777003756a923be
- 出典データセット
- uspto-grants-1976_08
- 特許番号
- US03975443
反応ノート
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