HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lawesson's reagent → 1-[4-(1-Hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinethione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lawesson's reagent | HCID 87949 | — |
| Reactant | 1-[4-(1-Hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinone | HCID 10314070 | — |
| Reactant | 2,4-Bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane | HCID 12732875 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | 1-[4-(1-Hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinethione | HCID 10359799 | 57.3% |
Reaction Steps
A mixture comprising 5 g of 1-[4-(1-hexahydroazepinyl)benzenesulphonyl]-2-pyrrolidinone, prepared as in Example 18 of the European Patent Application published under No. 0,033,578, and 3.13 g of Lawesson reagent (or 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane in 100 cm3 of dimethoxyethane is heated to reflux for 3 hours. The mixture is allowed to return to room temperature and is evaporated to dryness, and the residue is chromatographed on silica (eluant: benzene). 2 g of product are recovered. M.p. 168°-170° C. After crystallization in methanol, 1.5 g of expected product are obtained. M.p. 172°-173° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05037822 |
| Source dataset | uspto-grants-1991_08 |
| ORD ID | ord-6e3a5dd5f765421fb65cc03a736ba03d |
| Source note | uspto-grants-1991_08 |