HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfoxide → 2-Chlorobenzyl azide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfoxide | HCID 679 | — |
| Reactant | 2-Chlorobenzyl chloride | HCID 11906 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Solvent | Water | HCID 962 | — |
| Product | 2-Chlorobenzyl azide | HCID 12194602 | — |
Reaction Steps
Sodium azide (3.36 g, 51.1 mmol, Eq: 1.05) was charged in the reactor followed by DMSO (35.2 g, 32.0 ml) and Hunig's base (642 mg, 868 μl, 4.87 mmol, Eq: 0.1). The suspension was stirred for 10 Min. at 25° C. Then 1-chloro-2-(chloromethyl)benzene (8 g, 6.29 ml, 48.7 mmol, Eq: 1.00) was added dropwise over 60 min. (Tr=25° C.) and stirred at 25° C. until reaction completion (<2 h). The resulting white suspension was treated with water (1.6 g, 1.6 ml) and stirred for 45 Min. at R.T. The suspension was filtered and the filter cake was washed with DMSO (17.6 g, 16.0 ml) to give a colorless solution of 1-(azidomethyl)-2-chloro-benzene solution.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08741906B2 |
| Source dataset | uspto-grants-2014_06 |
| ORD ID | ord-3d6f7de359a64c738b31a2edc9ff0426 |
| Source note | uspto-grants-2014_06 |