HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → HCID 59751427, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | 648904-56-7 | HCID 5327043 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59751427 | HCID 59751427 | 73.2% |
Reaction Steps
Dissolve the compound of Example 3 (120 mg, 0.23 mmol) in dichloromethane (3 mL) and add isobutylchloroformate (38 μL, 0.30 mmol) dropwise. After stirring for 10 minutes, pour the reaction into vigorously stirred ether (10 mL) and filter. Dissolve the solids in dichloromethane (10 mL) and wash with saturated aqueous sodium bicarbonate. Dry the organic layer with sodium sulfate, filter and concentrate in vacuo. Chromatograph the residue on a SiO2 column eluting with methanol in dichloromethane (4%) to give 104 mg of the title compound (73%): mass spectrum (ion spray): m/z=618.4 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07399867B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-20b650a5825c4c1b808b4fc1cf51b68e |
| Source note | uspto-grants-2008_07 |