HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 67040418, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Reactant | HCID 67040855 | HCID 67040855 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 67040418 | HCID 67040418 | — |
Reaction Steps
To a solution of Example 239c (2.8 g, 6.8 mmol) in dichloromethane (40 mL) was added pyridine (1.1 g, 13.7 mmol) and 2,2,2-trichloroethyl chloroformate (1.7 g, 2.8 mmol). The mixture was stirred at room temperature for 72 h. The reaction was poured into water. The aqueous phase was extracted with ethyl acetate (2×). The combined organic phases were washed with water, brine, and dried over sodium sulfate, filtered and concentrated under vacuum giving the title compound. The residue was purified by silica gel chromatography eluting with hexane/ethyl acetate/methanol (80:15:5) to give the desired product (2.0 g, 53%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07910595B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-330233d200e94e51bc37989beafd6247 |
| Source note | uspto-grants-2011_03 |