HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1693200Generated: November 1, 2026
Cesium carbonate → Methyl 5-(difluoromethoxy)picolinate
https://huagongshe.com/reaction/1693200
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2-Chloro-2,2-difluoroacetophenone | HCID 238296 | — |
| Reactant | Methyl 5-hydroxypyridine-2-carboxylate | HCID 4715126 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Methyl 5-(difluoromethoxy)picolinate | HCID 57827732 | 22.9% |
Reaction Steps
Cesium carbonate (7.45 g) and 2-chloro-2,2-difluoroacetophenone (5.75 g) were added to a solution of methyl 5-hydroxypyridine-2-carboxylate (2.5 g) in DMF, and the mixture was stirred at 100° C. for three hours. The reaction solution was returned to room temperature. Aqueous ammonium chloride and ethyl acetate were added and the organic layer was separated. The organic layer was washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. The organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (760 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08158620B2 |
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| Source dataset | uspto-grants-2012_04 |
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| ORD ID | ord-76a93ea84f3f4de195519c7862de1a6b |
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| Source note | uspto-grants-2012_04 |
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