HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 69036806, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 69038734 | HCID 69038734 | — |
| Catalyst | 1,1-Dichloroethane | HCID 6365 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 69036806 | HCID 69036806 | — |
Reaction Steps
To 7.2 mmol 5-cyclopropanesulfonyl-2-hydroxy-benzoic acid in 20 ml dichloroethane containing a few drops of DMF was added dropwise 8.7 mmol oxalyl chloride. After stirring for 90 min at RT, the reaction mixture was cooled to 0° C. and then 144 mmol methanol was added, followed by 72 mmol pyridine, and stirring continued at RT for 1 h. The mixture was then washed with 1 M aq HCl, dried with Na2SO4, and concentrated in vacuo. The residue was chromatographed on silica gel (eluant: ethyl acetate/heptane gradient) to afford the title compound. MS (m/e): 255.2 ([M−H]−, 100%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07605163B2 |
| Source dataset | uspto-grants-2009_10 |
| ORD ID | ord-af4307c5c40f4aa79536325b6eb43d55 |
| Source note | uspto-grants-2009_10 |