Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Benzenesulfonyl chloride | HCID 7369 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | 1-Hydroxy-6-nitrobenzotriazole | HCID 152817 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | HCID 20300028 | HCID 20300028 | 53.6% |
Reaction Steps
In 1 N aqueous sodium hydroxide (45 ml) is dissolved 1-hydroxy-6-nitro-1,2,3-benzotriazole (7.2 g). To the solution is added dropwise benzenesulfonyl chloride (7.0 g) with stirring at room temperature and further are added thereto water (50 ml) and ethyl acetate (100 ml) and the mixture is stirred for 1 hour. The ethyl acetate layer is separated, dried over magnesium sulfate-charcoal, filtered and concentrated until it becomes about 30 ml. n-Hexane (50 ml) is thereto added and the mixture is allowed to stand. The precipitated crystals are separated by filtration and dried to give faint yellow prisms of 1-benzenesulfonyloxy-6-nitro-1,2,3-benzotriazole (6.8 g), melting point: 122°-124° C. The product is recrystallized from ethyl acetate-n-hexane to give a pure product: melting point: 124° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04242507 |
|---|
| Source dataset | uspto-grants-1980_12 |
|---|
| ORD ID | ord-e99f9d1d4a5d4ee4bb83db65fa9f4ce8 |
|---|
| Source note | uspto-grants-1980_12 |
|---|