HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Boron trifluoride etherate → 2-[1,3-Dithian-2-yl]-5-nitrobenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Boron trifluoride etherate | HCID 8000 | — |
| Edukt | 1,3-Propanedithiol | HCID 8013 | — |
| Edukt | Sulfuric acid magnesium salt (1:1) | HCID 24083 | — |
| Edukt | 3-Hydroxy-6-nitroisobenzofuran-1(3h)-one | HCID 522671 | — |
| Lösungsmittel | Chloroform | HCID 6212 | — |
| Produkt | 2-[1,3-Dithian-2-yl]-5-nitrobenzoic acid | HCID 13530282 | — |
Reaktionsschritte
To an ice-cooled mixture of the Compound 3a (5.00 g, 25.6 mmol) and propane-1,3-dithiol (2.92 g, 27 mmol) in chloroform (75 mL) was added boron trifluoride etherate (2 mL). The mixture was stirred and allowed to warm to room temperature. After stirring for 3 hours, most of the solid had dissolved. Magnesium sulfate was added to dry the solution, and stirring was continued overnight. Filtration and evaporation of the solvent afforded a light yellow solid. This material was triturated with butyl chloride to give the Compound 3b; m.p. 192°-194° C.; 1H NMR (CDCl3 +MeSO-d6 +D2O) δ1.8-2.3 (m, 2H, CH2CH2CH2), 2.9-3.2 (m, 4H, --CH2CH2CH2 --), 6.56 (s, 1H, --SCHS--), 7.6-8.8 (m, 3H, ArH).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04591587 |
| Quelldatensatz | uspto-grants-1986_05 |
| ORD ID | ord-f79e795ee5f84617bc5ef94fee4f486a |
| Quellennotiz | uspto-grants-1986_05 |