HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 22660821, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methanesulfonamide | HCID 72879 | — |
| Reactant | HCID 491098 | HCID 491098 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22660821 | HCID 22660821 | 57.5% |
Reaction Steps
Methanesulfonamide (0.0188 g, 0.198 mmol), sodium hydride, and the acid chloride of 49 (0.0083 g, 0.019 mmol) were reacted in dimethylformamide and dichloromethane according to the procedure described for example 8. The crude material was purified by reverse phase HPLC (C18 column, water/acetonitrile gradient containing 0.05% trifluoroacetic acid) to afford the product as a white solid (0.0055 g, 52%). 1H NMR (CDCl3) δ 8.68 (s, 1H), 8.17 (d, 1H, J=8.8 Hz), 7.91 (d, 1H, J=8.8 Hz), 7.69 (d, 2H, J=8.5 Hz), 7.48-7.37 (m, 5H), 7.24 (d, 2H, J=8.7 Hz), 5.18 (s, 2H), 4.57 (m, 1H), 3.34 (s, 3H), 2.34 (br m, 2H), 2.06 (br m, 4H), 1.85 (br m, 1H), 1.39 (br m, 3H); ESI-MS m/e 504.3 (M+1); HPLC purity (ELSD)>95%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06803374B2 |
| Source dataset | uspto-grants-2004_10 |
| ORD ID | ord-5fb3c26bd4f147d6aaa9eb9be99ef7e0 |
| Source note | uspto-grants-2004_10 |