HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 135430232, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 3-(7-Amino-1,1-dioxido-4h-1,2,4-benzothiadiazin-3-yl)-1-(5,5-dimethylhexyl)-4-hydroxy-1-methylnaphthalen-2(1h)-one hydrochloride | HCID 136397171 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 135430232 | HCID 135430232 | 75% |
Reaction Steps
A solution of Example 37B (0.374 g, 0.722 mmol), mesyl chloride (0.224 mL, 2.89 mmol), and pyridine (0.467 mL, 5.78 mmol) in acetone (15 mL) was stirred at 25° C. for 18 hours. The solution was partitioned between ethyl acetate and dilute citric acid and the layers were separated. The ethyl acetate layer was dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed on silica gel eluting with methylene chloride and 2.5% methanol in methylene chloride to give the desired product (0.302 g, 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07378414B2 |
| Source dataset | uspto-grants-2008_05 |
| ORD ID | ord-1aaec40180e44bcc8143e7736c80af0b |
| Source note | uspto-grants-2008_05 |