HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1-Hydroxybenzotriazole → [2-(3-Fluoro-phenyl)-ethoxy]-acetic acid methyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| Edukt | 2-[2-(3-Fluorophenyl)ethoxy]acetic acid | HCID 24769444 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | [2-(3-Fluoro-phenyl)-ethoxy]-acetic acid methyl ester | HCID 67099252 | 93% |
Reaktionsschritte
A solution of [2-(3-fluoro-phenyl)-ethoxy]-acetic acid (1.20 g, 6.05 mmol), EDCl (1.28 g, 6.66 mmol), HOBt (0.90 g, 6.66 mmol) and DIPEA (1.56 ml, 9.08 mmol) in methanol (4 ml) was stirred at 0° C. for 2 hours. The reaction mixture was brought to dryness, the residue was dissolved in CH2Cl2 and was washed twice with 1M NaOH and brine. The organic layers were dried over MgSO4, filtered, the solvent was removed under reduced pressure and the residue was purified by column chromatography (silica gel, EtOAc/heptane, 1:4) to yield the title compound (1.20 g, 5.6 mmol; 93%) as colorless liquid. MS: m/e=213.2 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07928106B2 |
| Quelldatensatz | uspto-grants-2011_04 |
| ORD ID | ord-6a1b498125b64f2abfa35e174679a1d2 |
| Quellennotiz | uspto-grants-2011_04 |