HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol, magnesium salt (2:1) → HCID 72357170, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol, magnesium salt (2:1) | HCID 164537 | — |
| Reactant | HCID 68743481 | HCID 68743481 | — |
| Product | HCID 72357170 | HCID 72357170 | 82.5% |
Reaction Steps
A solution of 4-methoxy-6-trifluoromethylpyran-2-one (2.7 g, 14 mmol) in a methanolic magnesium methanolate solution (8.5% Mg(OMe)2, 8.36 g, 8 mmol) was heated under reflux for 16 hours. The solution was concentrated and taken up in water and ethyl acetate, and the organic phase was brought to pH 5 by adding dilute hydrochloric acid. The organic phase was separated off, dried and concentrated. 1.5 g of crude product were obtained as a yellow oil. Kugelrohr distillation at 0.04 mbar and about 160° C. afforded methyl 6,6,6-trifluoro-3-methoxy-5-oxo-2-hexenoate (1.50 g, 6.6 mmol, 48%) as a pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07351851B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-0d3dbbf228c34a99b1b64c2cb8366de9 |
| Source note | uspto-grants-2008_04 |