化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → Dimethyl 2,2'-dithiobisbenzoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Dithiodibenzoic acid | HCID 8409 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Thionyl Chloride | HCID 24386 | — |
| 生成物 | Dimethyl 2,2'-dithiobisbenzoate | HCID 79574 | 50% |
反応手順
25 g (81.6 mmol) of dithiodibenzoic acid is refluxed in 60 ml of SOCl2 and 1.5 ml of dimethylformamide (DMF) for 3 hrs. Then the excess of SOCl2 is distilled off, and the residue is dissolved in CHCl3 and added dropwise to a solution of methanol (50 ml) and triethylamine (0.204 mol) in CHCl3 (300 l). After standing over night the reaction mixture is shaked with water and saturated K2CO3 solution. After drying the organic layer the solvent is evaporated and methanol is added to the residue (oil). 13.6 g (50%) of solid product is obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07901867B2 |
| 出典データセット | uspto-grants-2011_03 |
| ORD ID | ord-cad53b8c9b884337997cc19785bc4fe7 |
| 出典メモ | uspto-grants-2011_03 |