HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Sulfate → 65416-26-4
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Sulfate | HCID 6163 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | (3E)-4-(2,6,6-Trimethyl-1-cyclohexen-1-yl)-3-buten-2-ol | HCID 5373729 | — |
| Product | 65416-26-4 | HCID 6436993 | — |
Reaction Steps
74.0 g (0.48 mol) of diethyl sulphate were added dropwise to a suspension of β-ionol alcoholate [obtained from 65.8 g (0.34 mol) of β-ionol and 18.4 g (ca 0.44 mol) of 55%-60% sodium hydride in 600 ml of benzene] in such a manner that the temperature did not exceed 50° C. Subsequently, the mixture was stirred at reflux for 3 hours, cooled and worked-up as described in Example 1. Crude distillation of the crude product (72.0 g) gave 50.2 g of crude product which were subsequently purified by distillation over a 20 cm Widmer column. There were obtained 47.0 g (66.1%) of pure and olfactorily good β-ionyl ethyl ether 2 of boiling point 120°-122° C./10 mmHg.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04461309 |
| Source dataset | uspto-grants-1984_07 |
| ORD ID | ord-4aadb3bff7c24f07a3de8717809ccc14 |
| Source note | uspto-grants-1984_07 |