HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68814860, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 67200945 | HCID 67200945 | — |
| Product | HCID 68814860 | HCID 68814860 | — |
Reaction Steps
A solution of 3-hydroxy-1-(2,6,6-trimethyl-3-cyclohexen-1-yl)-1-butanone (2.00 g, 84% pure, 8.0 mmol) in pyridine (1.85 g, 23.4 mmol) was treated at 0° C. with ethyl chloroformate (1.24 g, 23.4 mmol). The reaction solution was stirred at room temperature for 36 hours, treated with aqueous 5% HCl and extracted twice with ether, washed with water, saturated aqueous NaHCO3, then with saturated aqueous NaCl, dried over Na2SO4 and concentrated. The oil thus obtained was purified by flash-chromatography (cyclohexane/AcOEt=98:2), using SiO2 (100 g). Yield: 2.06 g (78%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07589055B2 |
| Source dataset | uspto-grants-2009_09 |
| ORD ID | ord-ba3361b115994f36aaf5c38421caacf3 |
| Source note | uspto-grants-2009_09 |