HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 86624959, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methyl triflate | HCID 9526 | — |
| Reactant | HCID 59847703 | HCID 59847703 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 86624959 | HCID 86624959 | 80% |
Reaction Steps
To a stirred solution of 3.90 g (19.8 mmol) 9 and 70 ml dichloromethane were added 32.5 g (198 mmol) methyltriflate (Aldrich) drop wisely. The reaction mixture was stirred for 2.5 days at room temperature and diethylether was added. The desired compound precipitates and the solvent were decanted. The solid was washed extensively (ten times) with large amounts of diethylether. The solid was dried by use of oil pump vacuum and purified by (C-18) RP-column chromatography (acetonitril/water-gradient 1:99 to 80:20). The desired compound 10 was obtained in 80% yield (5.72 g, 15.84 mmol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08557776B2 |
| Source dataset | uspto-grants-2013_10 |
| ORD ID | ord-a148722d6a9d44cfa23c526279f4bb7e |
| Source note | uspto-grants-2013_10 |