HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 66580942, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 66581050 | HCID 66581050 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66580942 | HCID 66580942 | 97% |
Reaction Steps
To a solution of 2-bromo-N-[3-(morpholin-4-ylcarbonyl)-1-phenyl-1H-pyrazol-4-yl]benzenesulfonamide (30 mg; 0.06 mmol; 1.00 eq.) in THF (6 mL) is added sodium hydride (3 mg; 0.07 mmol; 1.20 eq.) and the reaction is stirred for 10 min before the addition of iodomethane (4 μL; 0.07 mmol; 1.10 eq.). After 12 h, DCM is added to the reaction mixture, ished with water (×2) and dried the organic phase over MgSO4 give 30 mg (97%) of the title compound as a white solid. 1H NMR (DMSO) δ 8.64 (s, 1H), 7.93-7.86 (m, 2H), 7.80-7.73 (m, 2H), 7.62-7.47 (m, 4H), 7.41-7.32 (m, 1H), 3.65-3.51 (m, 6H), 3.48-3.42 (m, 2H), 3.35 (s, 3H). HPLC (max plot) 89.7%; Rt 3.98 min. MS (ESI+): 507.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09073940B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-387abd6fa43d406c85541afc4264ae86 |
| Source note | uspto-grants-2015_07 |