HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 66661034, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Phenyl chloroformate | HCID 15891 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 66661062 | HCID 66661062 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 66661034 | HCID 66661034 | 79% |
Reaction Steps
To a mixture of the crude compound obtained in step b above (1400 mg) in dioxane (18 mL) and water (2 mL) was added phenyl chloroformate (0.9 mL, 7.16 mmol) and DIEA (1.6 mL, 8.95 mmol). The mixture was stirred at room temperature for 3 h and concentrated under reduced pressure. The residue was partitioned between water and EtOAc. The aqueous layer was extracted with EtOAc, the combined organic phases were dried and concentrated. The residue was purified by silica gel column chromatography to afford the title compound as a white solid (1165 mg, 79% yield, three steps).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08022092B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-4b911612e5cb4024976a1abb65264d55 |
| Source note | uspto-grants-2011_09 |