1,1'-Thiocarbonyldiimidazole → HCID 22139828、化合物
反応式
[C:1]([N:8]1[CH:12]=[CH:11]N=C1)(N1C=CN=C1)=[S:2].NC1[C:18]([Cl:19])=[CH:17][S:16]C=1>C1COCC1>[Cl:19][C:18]1[C:12]([N:8]=[C:1]=[S:2])=[CH:11][S:16][CH:17]=1参加物
4
実験手順
1.46 g of thiocarbonyldiimidazole are added to a solution of 1.1 g of 3-amino-4-chlorothiophene in 20 ml of anhydrous THF, and the mixture is stirred at room temperature for one hour. The solid is distilled off under reduced pressure, the residue is dissolved in ethyl acetate, the organic phase is treated twice with water in a separating funnel and then dried, and the solvent is again distilled off under reduced pressure. This gives 4-chloro-3-thienyl isothiocyanate as a dark oil which is then reacted further without further purification steps.
後処理
- distillationThe solid is distilled off under reduced pressure
- dissolutionthe residue is dissolved in ethyl acetate
- additionthe organic phase is treated twice with water in a separating funnel
- customdried
- distillationthe solvent is again distilled off under reduced pressure
- customThis gives 4-chloro-3-thienyl isothiocyanate as a dark oil which is then reacted further without further purification steps
出典と根拠
- ORDレコード
- ord-eb11950cf2bc42569f28c9f713bb2810
- 出典データセット
- uspto-grants-2010_07
- 特許番号
- US07763643B2
反応ノート
読み込み中…