HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 55266256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 3-Piperidinol, 1-methyl- | HCID 98016 | — |
| Catalyst | Methanesulfonyl chloride | HCID 31297 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 55266256 | HCID 55266256 | 325.1% |
Reaction Steps
To a solution of 3-hydroxy-N-methyl piperidine (2 cm3, 17.4 mmol) in dichloromethane (40 cm3) was added triethylamine (3.6 cm3, 26.05 mmol) and then methanesulfonyl chloride (1.5 cm3, 19:1 mmol). The reaction was then stirred for 3 h before a further aliquot (0.2 equiv., 3.47 mmol) of methanesulfonyl chloride was added. Stirring was continued for another 2 h at room temperature before the reaction was treated with water (60 cm3) and extracted into dichloromethane (40 cm3). The organic layer was washed with saturated aqueous sodium chloride solution (60 cm3) and dried over sodium sulfate before being evaporated under reduced pressure to afford (A) (2.18 g, 11.28 mmol, 65%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07838518B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-dbec53f4337a411aa8cc0d5a4fd55cf7 |
| Source note | uspto-grants-2010_11 |