Carbon Disulfide → HCID 14651794、化合物
反応式
[CH2:1]([C:8]#N)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[CH3:10][NH:11][CH2:12][CH2:13][NH2:14].C(=S)=S>C(OCC)(=O)C>[CH3:10][N:11]1[CH2:12][CH2:13][N:14]=[C:8]1[CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]参加物
5
反応条件
- 温度
- 125 °C
実験手順
14.207 g (113.46 mmoles) of heptyl cyanide, 10.726 g (144.69 mmoles) of N-methylethylenediamine and 0.5 ml of carbon disulfide were mixed and heated at 125° C. for 24 hours. The solution was cooled, diluted with ethyl acetate and extracted with dilute hydrochloric acid. The acidic solution was basified with sodium hydroxide and extracted with ethyl acetate. The organic extracts were treated with charcoal, filtered, concentrated and Kugelrohr distilled at 105° C./1.2 mm to give 19.73 g (77.3%) of the product.
後処理
- temperatureThe solution was cooled
- extractionextracted with dilute hydrochloric acid
- extractionextracted with ethyl acetate
- additionThe organic extracts were treated with charcoal
- filtrationfiltered
- concentrationconcentrated
- distillationKugelrohr distilled at 105° C./1.2 mm
出典と根拠
- ORDレコード
- ord-d6997c8cf6ed41e5a05bcb7568a6f02f
- 出典データセット
- uspto-grants-1991_07
- 特許番号
- US05030629
反応ノート
読み込み中…