HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86718262, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 86718260 | HCID 86718260 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86718262 | HCID 86718262 | — |
Reaction Steps
In 6 ml of toluene, 300 mg of Compound 8a-1 synthesized in Production Example 19 was dissolved. To the solution thus obtained, 235 μl of triethylamine and 122 μl of methanesulfonyl chloride were added, and the resulting mixture was stirred at room temperature for 1 hour. After the reaction, water was added to the reaction solution thus obtained, and extraction with ethyl acetate was carried out. The organic layer thus extracted was washed with an aqueous solution of hydrochloric acid, an aqueous solution of sodium hydrogen carbonate, and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled away, and the residue was then purified by silica gel column chromatography to obtain 378.3 mg of Compound 9a-1-1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09278966B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-1b21adf375e9400a914ed8f8f323d9bd |
| Source note | uspto-grants-2016_03 |