HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → HCID 4420006, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 13076189 | HCID 13076189 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 4420006 | HCID 4420006 | 95% |
Reaction Steps
A solution of 5.0 g 3-fluoro-8-isopropyl-10-piperazine-10,11-dihydrodibenzo(b,f)thiepin in 20 ml chloroform is stirred and treated dropwise with 2.2 g acetyl chloride. The mixture is then left overnight at room temperature. Then, the separated hygroscopic hydrochloride of the product is filtered with suction, suspended in water and the base released by an excess of 20% sodium hydroxide solution and isolated by extraction with chloroform. Processing of the extract yields 5.4 g (95%) crude base of 10-(4-acetylpiperazino)-3-fluoro-8-isopropyl-10,11-dihydrodibenzo(b,f)thiepin which crystallizes from a mixture of benzene and petroleum ether and melts in a pure state at 164.5°-166° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04243805 |
| Source dataset | uspto-grants-1981_01 |
| ORD ID | ord-6b7624d5faa64b6bb79735d521b55bf2 |
| Source note | uspto-grants-1981_01 |