HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 19369481, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 19369493 | HCID 19369493 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19369481 | HCID 19369481 | 57.3% |
Reaction Steps
After a mixture of 1.690 g (3.95 mmol) of 8-[3-(2-quinolinylmethoxy)benzylamino]-3,4-dihydro-2H-1,4-benzothiazin-3-one obtained in Example 95, 0.673 g (4.74 mmol) of CH3I, 1.311 g (9.5 mmol) of K2CO3, 0.129 g (0.4 mmol) of (n-Bu)4NBr and 50 ml of DMF was stirred at room temperature for 3 days, the solvent was distilled off under reduced pressure. Water was added to the residue, followed by extraction with CHCl3. The extract was washed with water, dried over MgSO4 and then concentrated. The residue was subjected to chromatography on a silica gel column. Subsequent to elution with CHCl3, recrystallization was conducted from an acetone-n-hexane mixed solvent, whereby 1.000 g of the title compound was obtained (yield: 57.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05885987 |
| Source dataset | uspto-grants-1999_03 |
| ORD ID | ord-21a864262b7b4ace9d2785168026cdfe |
| Source note | uspto-grants-1999_03 |