HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus sulfide (P2S5) → 2-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepine-5(4H)-thione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | Potassium Sulfide | HCID 162263 | — |
| Reactant | 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepin-5(4H)-one | HCID 13726363 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 2-(2-Chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepine-5(4H)-thione | HCID 13726364 | — |
Reaction Steps
To a solution of 16.6 g (0.06 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylnaphth[2,3-f][1,4]oxazepin-5(4H)-one in 150 ml of dry toluene was added a mixture of 8.6 g (0.045 mole) of phosphorus pentasulfide and 8.6 g of potassium sulfide which had been ground together. The reaction mixture was stirred and heated at reflux for 24 hr. The mixture was filtered hot and the filtrate concentrated under reduced pressure. Yellow solid, 6.5 g (35%) was obtained which was recrystallized from ethanol, m.p. 166°-168° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04810795 |
| Source dataset | uspto-grants-1989_03 |
| ORD ID | ord-0dbc9157fe2c4cafa47bcbb678872355 |
| Source note | uspto-grants-1989_03 |