HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 178462115, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 178462117 | HCID 178462117 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 178462115 | HCID 178462115 | — |
Reaction Steps
tert-Butyl trans-4-((R)-1-phenylethylcarbamoyl)cyclohexylcarbamate (Intermediate 41, 5.2 g) was dissolved in DCM (50 mL) to which TFA was added. The resulting mixture was stirred for 45 min at room temperature. LC-MS of material showed one major peak which corresponded to desired product. The reaction mixture was then concentrated to give a clear oil. The oil was then dissolved in diethyl ether (200 mL) to which HCl (2M solution in ether) (20 mL) was added. The resulting mixture was stirred at room temperature for 2 h, resulting in a white precipitate that was collected by filtration and washed with diethyl ether (4.1 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394858B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-60809547d0314ba799d54b8e32f7cf84 |
| Source note | uspto-grants-2013_03 |