HuagongsheHuagongshe Chemistry Print Report · For research reference only
m-Chloroperbenzoic acid → HCID 67745330, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | m-Chloroperbenzoic acid | HCID 70297 | — |
| Reactant | Potassium Bicarbonate | HCID 516893 | — |
| Reactant | HCID 57236704 | HCID 57236704 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67745330 | HCID 67745330 | 99.6% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
A solution of 20.3 g of 3-chloroperoxybenzoic acid (at 85%) in 300 cm3 of dichloromethane is added over 40 minutes to a solution, cooled to 0° C., of 25.4 g of 4,4-diphenyltetrahydrothiapyran in 130 cm3 of dichloromethane After stirring for 2 hours at 0° C., 250 cm3 of a 5% aqueous solution of potassium hydrogen carbonate are added to the mixture and it is then stirred for 15 minutes. The organic phase is again washed with 250 cm3 of a solution of potassium hydrogen carbonate and it is then dried over magnesium sulphate and concentrated to dryness (after verifying the absence of peroxides) under reduced pressure (2.7 kPa). 26.9 g of 4,4-diphenyltetrahydrothiapyran 1-oxide are obtained in the form of a white solid; melting point 122° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05484942 |
| Source dataset | uspto-grants-1996_01 |
| ORD ID | ord-fe804654e64b4eb09c0ce39b50629943 |
| Source note | uspto-grants-1996_01 |