Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 13006799 | HCID 13006799 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 22460335 | HCID 22460335 | 99% |
Reaction Steps
In 300 g of acetone was dissolved 26 g of the cyclohexylthio(4-hydroxyphenylthio)methane crude product in Synthesis Example 10. To this were added 21 g (0.15 mol) of potassium carbonate and 8.7 g (0.11 mol) of acetyl chloride. While heating in an oil bath at 70° C., the solution was ripened for 4 hours. At the end of ripening, the inorganic salt was filtered and washed with 50 g of acetone. The filtrate and wash liquid combined was concentrated, and the residue was dissolved in 300 g of dichloromethane and washed with 50 g of water. The organic layer was concentrated in vacuum again, obtaining 30 g of an oily product, which was used in the subsequent reaction without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06395446B1 |
|---|
| Source dataset | uspto-grants-2002_05 |
|---|
| ORD ID | ord-83648641293b45b69ebeae2eec4df068 |
|---|
| Source note | uspto-grants-2002_05 |
|---|