HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Sodium hydride → 3-(2-Methoxyethyl)thio-2-methyl-4-trifluoromethylbenzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2-Methoxyethanethiol | HCID 3014644 | — |
| Edukt | 3-Fluoro-2-methyl-4-(trifluoromethyl)benzoic acid | HCID 57457765 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 3-(2-Methoxyethyl)thio-2-methyl-4-trifluoromethylbenzoic acid | HCID 67158491 | — |
Reaktionsschritte
1.45 g (6.53 mmol) of 3-fluoro-2-methyl-4-trifluoromethylbenzoic acid were initially charged in 40 ml of DMF. 809 mg (20.2 mmol) of NaH were added a little at a time. After the evolution of gas had ceased, 1.20 g (13.1 mmol) of 2-methoxyethanethiol were added a little at a time. The mixture was stirred at RT for 10 minutes and then heated at 80° C. for 15 h. The reaction mixture was cooled and concentrated under reduced pressure, and for work-up water was added and the mixture was acidified with 1M HCl. The product precipitated and was removed by filtration. The product was then washed with water and n-heptane. What was isolated were 1.7 g of the pure product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07943551B2 |
| Quelldatensatz | uspto-grants-2011_05 |
| ORD ID | ord-cd88a9c7f9b54c5abfbba09d68fbec05 |
| Quellennotiz | uspto-grants-2011_05 |