HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonyl chloride → HCID 10167256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 68857586 | HCID 68857586 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 10167256 | HCID 10167256 | — |
Reaction Steps
The dried product from example 278B was dissolved in anhydrous pyridine (3 mL) at 0° C. for 30 minutes. Then methanesulfonyl chloride (50 μL, 6 mmoles) was injected. The reaction mixture was let to stand at room temperature for 3 hours. Then the reaction mixture was dried in vaccuo, dissolved in CH2Cl2 (4 mL), filtered and dried in vaccuo. The final residue was purified by HPLC to provide the titled compound. 1H NMR (500 MHz, DMSO-d6) δ8.95 (s, 1 H), 7.76 (s, 1 H), 7.27 (m, 7 H), 7.20 (m, 1 H), 7.04 (m, 1 H), 6.95 (m, 4 H), 6.71 (m, 1 H), 6.53 (m, 2 H), 4.06 (s, 2 H), 4.03 (s, 2 H), 3.92 (m, 1 H), 3.82 (m, 2 H), 2.91 (s, 3 H), 2.39 (s, 3 H), 2.04-2.29 (m, 3 H), 1.80 (m, 1 H); MS (APCI+) m/z 586 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06583180B2 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-e966dbd4fcf94c3c98b56c4ae9194853 |
| Source note | uspto-grants-2003_06 |