HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 23503188, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Sulfuryl chloride | HCID 24648 | — |
| Reactant | Piperidin-2-ylmethanol | HCID 94263 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23503188 | HCID 23503188 | 39% |
Reaction Steps
To a −78° C. hazy solution under a nitrogen atmosphere of racemic 2-piperidinemethanol (0.576 g, 5.00 mmol) and triethylamine (1.42 mL, 10.0 mmol) in anhydrous dichloromethane (30 mL) was added a solution of sulfuryl chloride (0.41 mL, 5.06 mmol) in anhydrous dichloromethane (30 mL) and the reaction was stirred for around 18 h from −78° C. to ambient temperature. The clear, yellow solution was washed with 1.0N HCl (2×25 mL) and brine (25 mL), dried over Na2SO4, concentrated in vacuo to a dark yellow oil, and purified by flash column chromatography (silica gel, ether) to afford the title product as a clear yellow oil (0.342 g, 39%). The proton NMR was identical to the desired product in procedure A, step 2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07402684B2 |
| Source dataset | uspto-grants-2008_07 |
| ORD ID | ord-72aa31f0723141a2903b551ccb6c6b78 |
| Source note | uspto-grants-2008_07 |