HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Methanesulfonic acid, 1H-benzotriazol-1-yl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Methanesulfonic acid, 1H-benzotriazol-1-yl ester | HCID 11745953 | — |
Reaction Steps
1-Hydroxy-1,2,3-benzotriazole (25.7 g) is suspended into water (50 ml) and thereto is added 1 N aqueous sodium hydroxide (180 ml). To the resulting solution is added dropwise methanesulfonyl chloride (14.0 ml) with stirring under ice-cooling and thereto is further added ethyl acetate (30 ml), and the mixture is stirred for 4 hours. The reaction mixture is extracted with ethyl acetate, and the extract is washed with water and dried over anhydrous magnesium sulfate. After drying, the solvent is distilled off and to the resulting residue is added petroleum ether, and the residue is cracked, filtered and dried to give 1-methanesulfonyloxy-1,2,3-benzotriazole (39.1 g), melting point: 88°-91° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04242507 |
| Source dataset | uspto-grants-1980_12 |
| ORD ID | ord-373c27c4570648709a8e7d39f2d185e4 |
| Source note | uspto-grants-1980_12 |