HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Methoxypropyl 4-methylbenzenesulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Methoxy-1-propanol | HCID 74116 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-Methoxypropyl 4-methylbenzenesulfonate | HCID 13522988 | — |
Reaction Steps
A solution of 3-methoxy-1-propanol (6 g, 65.24 mmol), triethylamine (27.5 mL, 195.7 mmol) and tosylchloride (18.85 g, 97.9 mmol) in methylene chloride (50 mL) is stirred for 3 h at room temperature under nitrogen. The mixture is poured into H2O, and the aqueous layer extracted twice with methylene chloride. The combined organic extracts are dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue is purified by flash column chromatography on silica gel (hexane/EtOAc 4/1) to afford the title compound as an orange oil: MS 261.9 [M+18]; Rt (HPLC, Nucleosil C18, 10:90-100:0 CH3CN/H2O+0.1% TFA within 5 min, then 100% CH3CN+0.1% TFA): 5.21 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07754727B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-906e4f55ecff4f838c68b95c7e87ac54 |
| Source note | uspto-grants-2010_07 |