HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrosylsulfuric acid → HCID 58062852, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrosylsulfuric acid | HCID 82157 | — |
| Reactant | HCID 58062859 | HCID 58062859 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58062852 | HCID 58062852 | 64.9% |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a solution of 1.81 g (12.81 mmol) nitrosylsulfuric acid in 1.5 ml water at 0° C. under nitrogene, was added dropwise a suspension of 463 mg (1.423 mmol) 2-benzyloxy-6-methoxy-4-trifluoromethyl-benzamide in 2.9 ml dichloromethane. The reaction mixture was stirred at 0° C. for 4 hours. The reaction mixture was poured over ice and extracted with dichloromethane. The combined organic layers were dried over sodium sulfate, filtered and evaporated. The crude solid was purified with flash column chromatography on silica (20 g) eluting with a gradient formed from n-heptane and ethyl acetate (0%=>100% in 15 minutes) to provide 431 mg (y: 64.9% yield) of the title compound as a white solid. MS (m/e): 325.1 (M−H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08080541B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-5f1e80a8c2024ee8b20d7b0df5cf1a5a |
| Source note | uspto-grants-2011_12 |