HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 22875137, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 22875136 | HCID 22875136 | — |
| Product | HCID 22875137 | HCID 22875137 | — |
Reaction Steps
To a solution of 0.101 g the intermediate from Step C in 1 mL of dichloromethane was added 1.0 mL of trifluoroacetic acid and maintained at RT for 30 min. The reaction mixture was evaporated to dryness, basified with 10% aqueous sodium carbonate solution (10 mL), and extracted with dichloromethane (3×5 mL). The combined organics were washed with brine (5 mL), dried over potassium carbonate, and concentrated. This material was dissolved in 2 mL of ethyl acetate and 0.10 mL of 4M HCl in EtOAc was added at 0° C. The precipitate was filtered under nitogen and washed with EtOAc/ether (1:1) and dried to give 62 mg of the product as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05536716 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-d230016c541c40efa41e74cfee40db29 |
| Source note | uspto-grants-1996_07 |