HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 10804488, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 2,4-Di-tert-butylphenol | HCID 7311 | — |
| Reactant | Tetrahydrothiopyran-4-one | HCID 66173 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 10804488 | HCID 10804488 | 74% |
Reaction Steps
A mixture consisting of 17 g (0.082 mol) of 2,4-di-tert-butylphenol, 4.8 g (0.041 mol) of tetrahydrothiopyran-4-one and 5 ml of acetic acid is melted together and is then saturated, with stirring, with hydrochloric acid gas at 40-45° C. After stirring for 12 hours at room temperature, the reaction mixture is diluted with toluene and washed with water, sodium chloride solution and sodium hydrogencarbonate solution. The organic phase is dried over magnesium sulfate and concentrated on a rotary-evaporator. The residue is crystallised from methanol, affording 9.2 g (74%) of 2,4-di-tert-butyl-6-(3,6-dihydro-2H-thiopyran-4-yl)phenol, m.p. 115-119° C. (compound (104), Table 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05932642 |
| Source dataset | uspto-grants-1999_08 |
| ORD ID | ord-ffc4dd7cf3a2456c838dabc00fba3b55 |
| Source note | uspto-grants-1999_08 |