HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → Methyl 4-amino-3-ethynylbenzoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| Edukt | HCID 59800132 | HCID 59800132 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Methyl 4-amino-3-ethynylbenzoate | HCID 640700 | 100,1% |
Reaktionsschritte
1.9 g (7.7 mmol) of methyl 4-amino-3-trimethylsilylethynylbenzoate were initially charged in 20 ml of tetrahydrofuran (THF). At from 5° C. to 8° C., 8.45 ml (8.5 mmol) of tetrabutylammonium fluoride solution (1 M in THF) were added dropwise within 5 minutes. After 25 mm at 2° C., 438 ml of acetic acid were added. After addition of water and extraction with dichloromethane, and after removal of the solvent, 1.35 g of methyl 4-amino-3-ethynylbenzoate were obtained. HPLC method as in example 1.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08232395B2 |
| Quelldatensatz | uspto-grants-2012_07 |
| ORD ID | ord-4929724427e04fcea22ea5b391f5bda6 |
| Quellennotiz | uspto-grants-2012_07 |