HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Dimethylformamide → Dimethyl 2,2'-dithiobisbenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Dimethylformamide | HCID 6228 | — |
| Edukt | Dithiodibenzoic acid | HCID 8409 | — |
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Potassium Carbonate | HCID 11430 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Lösungsmittel | Thionyl Chloride | HCID 24386 | — |
| Produkt | Dimethyl 2,2'-dithiobisbenzoate | HCID 79574 | 50% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07901867B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-cad53b8c9b884337997cc19785bc4fe7 |
| Quellennotiz | uspto-grants-2011_03 |