HuagongsheHuagongshe Chemistry Print Report · For research reference only
(Diethylamino)sulfur trifluoride → HCID 86693333, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| Reactant | HCID 86693330 | HCID 86693330 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86693333 | HCID 86693333 | 57% |
Reaction Steps
To a solution of ethyl 4-hydroxy-9-iodo-4-methyl-4,5-dihydrobenzo[b]pyrazolo[1,5-d][1,4]oxazepine-2-carboxylate (350 mg, 0.85 mmol, 1.00 equiv) in dichloromethane (5 mL) was added diethylaminosulfur trifluoride (271 mg, 1.68 mmol, 2.00 equiv) at 0° C. After being stirred overnight at room temperature the resulting mixture was washed with water, extracted with dichloromethane, 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 200 mg (57%) of the titled compound as a white solid; LC-MS (ES, m/z) 417 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034866B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-d4728d671dff435d8d85b4e207408c69 |
| Source note | uspto-grants-2015_05 |