HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → HCID 15291091, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | 18-Crown-6 | HCID 28557 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | 2-(Chloromethyl)-4-isopropyl-6-methoxybenzo[D]isothiazol-3(2H)-one 1,1-dioxide | HCID 9995173 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 15291091 | HCID 15291091 | 26% |
Reaction Steps
A solution of 18-crown-6 ether (0.60 g) and benzene (60 mL) was heated under reflux with a water separator for 1 hour, then cooled to room temperature. 2-Chloromethyl-4-isopropyl-6-methoxysaccharin (3.03 g) and sodium azide (0.65 g) were added, and the mixture was stirred for a week at room temperature, then chromatographed on a column of silica gel (silica gel 60, 83 g) using benzene as eluant. The fractions containing the product, which were identified by thin layer chromatography, were combined and concentrated affording 2-azidomethyl-4-isopropyl-6-methoxysaccharin as a solution in benzene (250 mL).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05464852 |
| Source dataset | uspto-grants-1995_11 |
| ORD ID | ord-1d4838076b604dfe911e87f95da97d89 |
| Source note | uspto-grants-1995_11 |