HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → (S)-1-(3,5-Dichloropyridin-4-yl)ethyl methanesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | (S)-1-(3,5-Dichloropyridin-4-yl)ethanol | HCID 66831621 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (S)-1-(3,5-Dichloropyridin-4-yl)ethyl methanesulfonate | HCID 86647459 | — |
Reaction Steps
Dissolve (S)-1-(3,5-dichloropyridin-4-yl)ethanol (5.02 g, 26.14 mmol) in dichloromethane (DCM, 100 mL) and cool the flask in an ice bath. Add triethylamine (TEA, 3.5 mL, 25.11 mmol) followed by the dropwise addition of methanesulfonyl chloride (2.2 mL, 28.42 mmol). Remove the ice bath and allow the reaction to warm to RT. After 4 hours, quench the reaction with water (100 mL) and separate layers. Extract the aqueous layer with DCM (50 mL) followed by 20% isopropyl alcohol (IPA)/chloroform (50 mL). Combine the organic extracts, dry over anhydrous sodium sulfate, filter and concentrate in vacuo. Yield: 7.15 g, (100%). MS (ES) m/z 270 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268869B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-15f610aa2a3e45548112c5ad14e2000b |
| Source note | uspto-grants-2012_09 |