HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → 7-Chloro-3,5-dihydrobenzo[e][1,4]oxazepine-2(1H)-thione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | 7-Chloro-3,5-dihydrobenzo[e][1,4]oxazepin-2(1H)-one | HCID 84048199 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 7-Chloro-3,5-dihydrobenzo[e][1,4]oxazepine-2(1H)-thione | HCID 86679710 | 107.5% |
Reaction Steps
To a suspension of 7-chloro-3,5-dihydrobenzo[e][1,4]oxazepin-2(1H)-one (3.01 g, 15.2 mmol) in tetrahydrofurane (102 ml) was added 2,4-bis-(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (3.45 g, 8.53 mmol) at room temperature. The reaction mixture was heated at reflux for 4 h. After cooling to room temperature the solvent was evaporated and the residue was crystallized from hot ethanol to give the title compound (1.96 g, 60%) as light yellow solid. MS m/e: 211.6 ([M−H]−).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08828989B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-2f39995c16374d908b14b95082549e1d |
| Source note | uspto-grants-2014_09 |