反応式
[CH3:1][N:2]([CH2:4][C:5]1[S:6][CH:7]=[C:8]([CH2:10][S:11][CH2:12][CH2:13][NH2:14])[N:9]=1)[CH3:3].Cl.[CH3:16][N:17]=[C:18](SC)[S:19][CH3:20]>C(O)C>[CH3:16][NH:17][C:18](=[N:14][CH2:13][CH2:12][S:11][CH2:10][C:8]1[N:9]=[C:5]([CH2:4][N:2]([CH3:1])[CH3:3])[S:6][CH:7]=1)[S:19][CH3:20]参加物
実験手順
Two g. of 2-dimethylaminomethyl-4-(2-aminoethyl)thiomethylthiazole, 25 ml. of denatured ethanol, 0.72 ml. of concentrated hydrochloric acid and 1.16 g. of methylcarbonimidodithioic acid, dimethyl ester, were added to a flask and heated under reflux for 16 hours. The reaction mixture was then evaporated to an oily residue under vacuum, and the residue was taken up in 25 ml. of water and extracted with two 15 ml. portions of diethyl ether. The aqueous layer was cooled and 3 ml. of 50% aqueous sodium hydroxide was added. The aqueous solution was then extracted with two 20 ml. portions of diethyl ether, and the extract was evaporated to dryness under vacuum to obtain 2.0 g. of crude product, which was identified by its mass spectrum, showing a molecular ion of weight 318, and by its nuclear magnetic resonance spectrum; 'H NMR (CDCl3) δ7.07 (s, 1H), 3.87 (s, 2H), 3.75 (s, 2H), 3.42 (t, 2H), 2.75 (m, 2H) and 2.33 (s, 9H).
後処理
- temperatureheated
- temperatureunder reflux for 16 hours
- customThe reaction mixture was then evaporated to an oily residue under vacuum
- extractionof water and extracted with two 15 ml
- temperatureThe aqueous layer was cooled
- additionof 50% aqueous sodium hydroxide was added
- extractionThe aqueous solution was then extracted with two 20 ml
- customportions of diethyl ether, and the extract was evaporated to dryness under vacuum
- customto obtain 2.0 g
出典と根拠
- ORDレコード
- ord-72cdfc7aea654aea82942ffa9d8ee6e6
- 出典データセット
- uspto-grants-1986_05
- 特許番号
- US04587344
関連ノート
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