HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 21922548, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 22565205 | HCID 22565205 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 21922548 | HCID 21922548 | 77.1% |
Reaction Steps
To a mixed solution of the compound obtained in Step 1 (2.00 g), chloroform (9.5 ml) and water (9.5 ml) was added trifluoroacetic acid (13.5 ml) under cooling with ice water. The reaction mixture was stirred at room temperature for 4 hours, adjusted to pH 8 with saturated aqueous solution of sodium hydrogencarbonate and extracted with methylene chloride. The organic layer was dried over anhydrous sodium sulfate and thereafter the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=2:1) to obtain the title compound (1.27 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07122662B2 |
| Source dataset | uspto-grants-2006_10 |
| ORD ID | ord-8c4ebdefedbc4d9c8e083cbba4db2424 |
| Source note | uspto-grants-2006_10 |