HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86639397, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Propargyl alcohol | HCID 7859 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86639398 | HCID 86639398 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86639397 | HCID 86639397 | 129.4% |
Reaction Steps
To a mixed solution of 150 ml of DMF, 12.7 g of 2-chloro-4,5-difluorobenzoic acid 2-propynyl ester and 3.4 g of propargyl alcohol, 2.4 g of 60% sodium hydride (oily) was added under ice cooling. After stirring at room temperature overnight, the reaction mixture was added with hydrochloric acid and extracted with ethyl acetate. The obtained organic layer was washed in turn with water and saturated brine, dried over magnesium sulfate and then concentrated under reduced pressure. The obtained residue was subjected to silica gel column chromatography, and 19 g of 2-chloro-5-fluoro-4-(2-propynyloxy)benzoic acid 2-propynyl ester was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07999136B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-118a2b1bc5b847fb865c3b5a8a955fbe |
| Source note | uspto-grants-2011_08 |