HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 3-(Methylthio)propyl 4-methylbenzenesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | 3-(Methylthio)-1-propanol | HCID 10448 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-(Methylthio)propyl 4-methylbenzenesulfonate | HCID 15310998 | — |
Reaction Steps
To a mixture of 3-methylthio-1-propanol (17) (5.0 g, 47.1 mmol), pyridine (7.43 g, 94.0 mmol) and CHCl3 (47 mL) cooled in an ice bath, tosyl chloride (13.47 g, 70.6 mmol) was added in portions with stirring. The mixture was allowed to warm to room temperature after 1 hour and stirring was continued for an additional 15 hours. The mixture was diluted with CH2Cl2 (200 mL), washed with water (2×100 mL), and the organic phase as dried (Na2SO4). The solvent was evaporated and the resulting yellow oil purified by column chromatography (silica gel, 15 wt % ether/hexanes, 50 wt % ether/hexanes), to give a colorless oil (10.5 g, 86 wt %), namely 3-methylthio-1-propanol tosylate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06552103B1 |
| Source dataset | uspto-grants-2003_04 |
| ORD ID | ord-498fd601d67d42c68ce69cb1421edd57 |
| Source note | uspto-grants-2003_04 |