HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → HCID 19610735, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | 1,3-Propanedithiol | HCID 8013 | — |
| Reactant | 1-Azabicyclo(2.2.2)octan-3-one, hydrochloride (1:1) | HCID 102019 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 19610735 | HCID 19610735 | 100% |
Reaction Steps
A mixture of 3-quinuclidinone hydrochloride (10 g, 62 mmol), 1,3-propanedithiol (13.4 g, 124 mmol), acetic acid (40 ml), and methanesulfonic acid (2 ml) was refluxed overnight. Most of the acetic acid was evaporated, 200 ml of water was added, and the solution was washed twice with ether. The pH of the solution was adjusted to basic by the addition of 1 M aqueous sodium hydroxide and the product was extracted with two portions of ethyl acetate. Drying over magnesium sulfate and evaporation of the solvent gave the title compound (13.3 g, 61.9 mmol, 100%) as a colorless solid 71-72° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05981539 |
| Source dataset | uspto-grants-1999_11 |
| ORD ID | ord-d29afeed90484caea95f5bda3add59bc |
| Source note | uspto-grants-1999_11 |