HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Methyl formate → (Z)-methyl 2-(hydroxymethylene)butanoate
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Methyl formate | HCID 7865 | — |
| Edukt | Methyl butyrate | HCID 12180 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Lösungsmittel | 1,2-Dimethoxyethane | HCID 8071 | — |
| Produkt | (Z)-methyl 2-(hydroxymethylene)butanoate | HCID 22056702 | 46,2% |
Reaktionsschritte
To a suspension of NaH (7.99 g, 200 mmol) in DME (100 mL) was added a mixture of methyl butyrate (5.1 g, 49.9 mmol) and methyl formate (17.99 g, 300 mmol) in DME (100 mL) dropwise at 0° C. under nitrogen. The mixture was stirred at room temperature overnight, and then filtered through a pad of celite. To the filtrate was added ether (200 mL), and let the suspension stand for 4 h. The solid was collected by filtration, washed with diethyl ether and dried in vacuo to afford the title compound (3 g, 23.05 mmol). LCMS: rt=1.108 min, [M+H+]=130
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08637536B2 |
| Quelldatensatz | uspto-grants-2014_01 |
| ORD ID | ord-2c088e74e59c4baea156540dfdf371c7 |
| Quellennotiz | uspto-grants-2014_01 |