HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 86730079, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Benzenesulfonyl chloride, 3,4-dichloro- | HCID 7383 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Tert-butyl (piperidin-4-ylmethyl)carbamate | HCID 723429 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86730079 | HCID 86730079 | 99.5% |
Reaction Steps
To a solution of 3,4-dichlorobenzene-1-sulfonyl chloride (470 mg, 1.91 mmol) was added tert-butyl piperidin-4-ylmethylcarbamate (410 mg, 1.91 mmol), followed by triethylamine (0.267 mL, 1.91 mmol). The reaction mixture was stirred for 16 h then diluted with DCM. The organic phase was washed with 1 N HCl, H2O, and brine, dried over Na2SO4, and then filtered. The solvent was evaporated under reduced pressure and the residue was purified on a 24 g cartridge using 0 to 100% EtOAc in hexanes and then 0 to 20% MeOH in DCM to yield Intermediate 9A (0.80 g, 1.9 mmol, 99% yield). LC-MS (ESI) 324.1. (M+H-Boc), RT=1.55 min (Method B).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394260B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-d5d54de44e4a4441a289802063efa1f5 |
| Source note | uspto-grants-2016_07 |