HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2'-Nitrobiphenyl-4-yl sulfamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chlorosulfamic acid | HCID 24499 | — |
| Reactant | 2,6-Di-tert-butyl-4-methylpyridine | HCID 98898 | — |
| Reactant | 4-Hydroxy-2'-nitrobiphenyl | HCID 15541112 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2'-Nitrobiphenyl-4-yl sulfamate | HCID 9904187 | 100.9% |
Reaction Steps
108 mg of 2′-nitrobiphenyl-4-ol was dissolved in 9.5 ml of methylene chloride, and 312 mg of 2,6-di-tert-butyl-4-methylpyridine and 347 mg of sulfamoyl chloride were successively added thereto under cooling with ice, followed by stirring at room temperature for 5 hours. After water was added to the reaction mixture, the product was extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. After the solvent was distilled off, the resulting crude product was purified by TLC (using a 1:1 mixture of ethyl acetate and hexane as the developing solvent) to obtain 149 mg of 2′-nitrobiphenyl-4-yl sulfamate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06762205B1 |
| Source dataset | uspto-grants-2004_07 |
| ORD ID | ord-08abfe412c9a4c429c4a6c61217c911b |
| Source note | uspto-grants-2004_07 |