HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroformate → HCID 57888831, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 66759036 | HCID 66759036 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 57888831 | HCID 57888831 | 94.1% |
Reaction Steps
A solution of (R)-4-(4-chlorophenyl)-3,3-dimethylpiperidin-4-ol (1.96 g, 8.18 mmol) in Pyridine (20 mL) was cooled to 0° C., then treated with the dropwise addition of ethyl chloroformate (0.942 mL, 9.81 mmol), causing a color change to orange. The mixture was allowed to come to room temperature and stirred over night. The reaction was concentrated in-vacuo, and the residue was taken up in ethyl acetate, washed 3× with 1M NaOH, 3× with 1M HCl, once with brine, dried over sodium sulfate, and concentrated in-vacuo to yield the title compound (2.4 g, 7.70 mmol, 94% yield). The residue was used as-is in the next step. MS (ESI+)=334, (M+Na)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07985861B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-b4f07f67c97d45079a7d15380cac2ddb |
| Source note | uspto-grants-2011_07 |