HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus sulfide (P2S5) → 7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | Potassium Sulfide | HCID 162263 | — |
| Reactant | 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)one | HCID 13726296 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 7-Chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepine-5(4H)-thione | HCID 13726301 | 86.1% |
Reaction Steps
To a solution of 20 g (0.07 mole) of 7-chloro-2-(2-chloroethyl)-2,3-dihydro-4-methyl-1,4-benzoxazepin-5(4H)-one in 200 ml of toluene was added a mixture of 9.55 g (0.05 mole) of phosphorus pentasulfide and 9.5 g of potassium sulfide which had been ground together. The reaction mixture was filtered and the filtrate concentrated under reduced pressure to give a yellow solid. Recrystallization from absolute ethanol gave 12.5 g (68%) of the product, m.p. 102°-104° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04705853 |
| Source dataset | uspto-grants-1987_11 |
| ORD ID | ord-91322b8531194d68880ec53ef89df07f |
| Source note | uspto-grants-1987_11 |