HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 24801301, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 24801299 | HCID 24801299 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 24801301 | HCID 24801301 | — |
Reaction Steps
A mixture of 0.10 g (0.247 mmol) [7-(4-aminomethyl-phenyl)-benzooxazol-2-yl]-(3,4,5-trimethoxy-phenyl)-amine (example 29) and 0.037 g (0.32 mmol) methanesulfonyl chloride in 4 ml pyridine is stirred for 1.5 h at room temperature. Then the reaction mixture is poured on water and extracted 3× with EtOAc. The combined organic layers are washed with 0.1N NaOH solution and water, dried over MgSO4, filtered and the filtrate is concentrated in vacuo and co-evaporated twice with toluene. The residue is purified by crystallisation from dichloromethane to afford the title compound as off-white crystals. Rt=2.20 min (Waters Symmetry C8, 2.1×50 mm, detection 210-250 nM, 5% to 100% CH3CN in H2O in 2 min+0.05% TFA, flow rate 1.0 ml/min); MS: 474 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08629168B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-a0fdb7748a4c438280fc514f3be66ee6 |
| Source note | uspto-grants-2014_01 |