HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl orthoformate → HCID 15114404, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl orthoformate | HCID 31214 | — |
| Edukt | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Edukt | 2-Bromo-5-(trifluoromethyl)benzaldehyde | HCID 7018047 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Produkt | HCID 15114404 | HCID 15114404 | 71% |
Reaktionsschritte
Step AJ (1): 2-Bromo-5-(trifluoromethyl)benzaldehyde (1069 mg, 4.975 mmol) was dissolved in a mixture of methanol (20 mL) and triethylorthoformate (20 mL). p-Toluenesulfonic acid monohydrate (180.0 mg, 0.946 mmol) was added and the reaction mixture was stirred under reflux for 5 h. The reaction was quenched with aqueous NaHCO3 and extracted with DCM. The combined organic phases were dried over Na2SO4, filtered and concentrated in vacuum at the temperature, not exceeding 35° C. The residue was purified by silica gel chromatography to give 1-bromo-2-(dimethoxymethyl)-4-methoxybenzene (1060 mg, 71%) as a colorless oil. LC-MS (M−OCH3)+=267.23.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07772221B2 |
| Quelldatensatz | uspto-grants-2010_08 |
| ORD ID | ord-25ca6c9a1559491c99e95eb8418e6fef |
| Quellennotiz | uspto-grants-2010_08 |