HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 68489720, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 68491393 | HCID 68491393 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 68489720 | HCID 68489720 | 62% |
Reaction Steps
Ethyl chlorocarbonate (32 mL, 336 mmol) was added to a toluene (200 mL) solution of the compound obtained in Example 1 (21.0 g, 56 mmol), and the mixture was refluxed while heating for 6 hours. The mixture was allowed to cool in the air, and the reaction mixture was added to a saturated aqueous sodium hydrogencarbonate solution to allow the separation of an organic layer. The organic layer was washed with a saturated sodium chloride solution and dried over anhydrous sodium sulfate, the solvents were then distilled off under a reduced pressure, and the residue was purified by column chromatography (hexane:ethyl acetate=19:1), to give 15.0 g (62%) of the captioned compound in the form of an oily product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08377967B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-104f4fdd6ea14a8e9acd95e614d01dfb |
| Source note | uspto-grants-2013_02 |