HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trimethylsilyldiazomethane → 4-Fluoro-3-methoxy-4-methylpent-2-enenitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trimethylsilyldiazomethane | HCID 167693 | — |
| Reactant | 4-Fluoro-4-methyl-3-oxopentanenitrile | HCID 86653507 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | 4-Fluoro-3-methoxy-4-methylpent-2-enenitrile | HCID 86653516 | 91% |
Reaction Steps
To a stirred solution of 4-fluoro-4-methyl-3-oxopentanenitrile (1 g, 7.75 mmol) in dry diethyl ether (150 mL) at 0° C., was added dropwise (trimethylsilyl)diazomethane (4.65 mL of a 2.0 M solution in diethyl ether, 9.30 mmol). After warming to room temperature the reaction mixture was stirred for a further 15 h. The reaction mixture was concentrated under reduced pressure to afford 4-fluoro-3-methoxy-4-methylpent-2-enenitrile as a yellow oil (1 g, 91%) which was taken on to the next step without further purification. 1H NMR (300 MHz, CDCl3) δ 4.89 (s, 1H), 4.23 (s, 3H), 1.47 (d, J=21 Hz, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08969587B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-ff1861f4b5e14663b83fd258e3b576cd |
| Source note | uspto-grants-2015_03 |