HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Toluenesulfonyl chloride → 3-[(tert-Butoxycarbonyl)amino]propyl 4-methylbenzene-1-sulfonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Toluenesulfonyl chloride | HCID 7397 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | tert-butyl N-(3-hydroxypropyl)carbamate | HCID 3838134 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 3-[(tert-Butoxycarbonyl)amino]propyl 4-methylbenzene-1-sulfonate | HCID 13120302 | 82% |
Reaction Steps
3-t-Butoxycarbonylaminopropanol (10.0 g) is dissolved in methylene chloride (100 ml) and thereto are added triethylamine (8.66 g) and tosyl chloride (16.3 g) with stirring under ice cooling. The mixture is stirred at room temperature overnight. The reaction mixture is concentrated and the residue is dissolved in water-ethyl acetate, and the organic layer is separated, washed with an aqueous saturated saline solution, dried over sodium sulfate, and then distilled off the solvent. The residue is purified with a silica gel column chromatography to give 3-t-butoxycarbonylaminopropyl tosylate (15.37 g) as pale yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06388078B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-89207e1eb2fe41e8af96b387045b65f6 |
| Source note | uspto-grants-2002_05 |