HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Sulfate → HCID 22818969, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Sulfate | HCID 6163 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | HCID 20434993 | HCID 20434993 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22818969 | HCID 22818969 | 55.4% |
Reaction Steps
6 g of potassium hydroxide, dissolved in a little water, are added dropwise to 36.85 g (0.1 mole) of 1-(4'-chloro-4-biphenylyloxy)-3,3-dimethyl-1-(imidazol-1-yl)-butan-2-one in 50 ml of dimethylsulphoxide. The mixture is subsequently stirred for a short time and 16 g (0.11 mole) of diethyl sulphate are then added dropwise. During this addition, the temperature of the reaction mixture is kept at about 40° C. and thereafter it was kept at 80° C. for 1/2 hour. It was allowed to cool, water is added and the crystalline precipitate is filtered off and recrystallised from petroleum ether. 22 g (50% of theory) of (E)-1-(4'-chloro-4-biphenylyloxy)-3,3-dimethyl-2-ethoxy-1-(imidazol-1-yl)-1-butene of melting point of 112°-113° C. are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04489085 |
| Source dataset | uspto-grants-1984_12 |
| ORD ID | ord-0aad7f92a3084132b916c0c587172c60 |
| Source note | uspto-grants-1984_12 |