HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → Benzoic acid, 4-[(methylsulfonyl)oxy]-, methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methylparaben | HCID 7456 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Benzoic acid, 4-[(methylsulfonyl)oxy]-, methyl ester | HCID 10466383 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
4-Hydroxy-benzoic acid methyl ester (3.19 g, 21 mmol) was dissolved together with pyridine (1.97 g, 25 mmol) in dry THF (20 mL) and after cooling down to 0° C., methanesulfonyl chloride (2.29 g, 20 mmol) was added dropwise. The ice bath was removed and mixture was stirred at r.t. for 5 h. After diluting with DCM and extraction with water and aq. HCl (2N), the organic layer was dried (MgSO4) and evaporated to afford the crude but highly pure product as a solid which was used in the next step without further purification (4.38 g, 95.1%). 1H NMR (400 MHz, CDCl3): δ 8.07-8.09 (d, 2H), 7.32-7.34 (d, 2H), 3.90 (s, 3H), 3.16 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181181B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-7ed561784c2f4d99b6011ffce2183adf |
| Source note | uspto-grants-2015_11 |