HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 86693320, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | HCID 86693321 | HCID 86693321 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86693320 | HCID 86693320 | 29% |
Reaction Steps
A suspension of ethyl 9-bromo-4-hydroxy-4,5-dihydrobenzo[2,3]oxepino[4,5-d]thiazole-2-carboxylate (500 mg, 1.35 mmol, 1.00 equiv), Ag2O (1.247 g, 4.00 equiv), and iodomethane (763 mg, 5.38 mmol, 4.00 equiv) in dichloromethane (5 mL) was stirred for 3 h at 50. The reaction was quenched with 10 mL of brine, extracted with ethyl acetate, dried over anhydrous sodium sulfate, and concentrated under vacuum. The residue was purified by a silica gel column with ethyl acetate/petroleum ether (1:20) to give 150 mg (29%) of the titled compound as a white solid; LC-MS (ES, m/z) 384, 386[M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034866B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-3e566723d68d42e2a7e86bbb836d690b |
| Source note | uspto-grants-2015_05 |