反応式
[SH:1][C:2]1[S:3][CH2:4][CH2:5][N:6]=1.CCN(CC)CC.[C:14](Cl)([Cl:16])=[O:15].CCOCC>C1COCC1.C1(C)C=CC=CC=1>[S:1]=[C:2]1[N:6]([C:14]([Cl:16])=[O:15])[CH2:5][CH2:4][S:3]1参加物
7
反応条件
- 温度
- 5 °C
実験手順
A solution of 2-mercaptothiazoline (2.0 g, 0.0168 mmol) and Et3N (2.9 ml, 0.021 mol) in THF (30 ml) was added dropwise to a solution of phosgene (2.37 g, 0.0239 mol) in toluene (12 ml) at 5° C. for 7 min. The mixture was stirred at 5° C. for 5 min and then filtered to remove the precipitate. The filtrate was evaporated in vacuo to give a crystalline residue. To the residue was added ether (10 ml) and the ether was evaporated in vacuo. This operation was repeated twice. 2-Thioxo-3-thiazolidinecarbonyl chloride (2,0 g) was obtained as a solid. 65.5% yield. IR (Nujol).
後処理
- filtrationfiltered
- customto remove the precipitate
- customThe filtrate was evaporated in vacuo
- customto give a crystalline residue
- customthe ether was evaporated in vacuo
出典と根拠
- ORDレコード
- ord-38183b71ef304e3ba36e202eb35f3851
- 出典データセット
- uspto-grants-1987_02
- 特許番号
- US04643991
関連ノート
読み込み中…