HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 86663079, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | HCID 86663078 | HCID 86663078 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 86663079 | HCID 86663079 | 76.8% |
Reaction Steps
2-chloro-5-(2-methoxyphenyl)pyridin-4-amine (7.5 g, 31.96 mmol) was dissolved in glacial acetic acid (200 mL) and concentrated sulfuric acid (1 mL). A solution of t-butylnitrite (11.39 mL, 95.87 mmol) in 10 mL of acetic acid was added drop wise and stirred for 30 minutes. The reaction mixture was concentrated under reduced pressure, dissolved in methylene chloride. The reaction mixture was dried over sodium sulfate, concentrated and the residue was purified by silica column using hexanes and ethyl acetate as eluent to give 5.0 g of title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09359549B2 |
| Source dataset | uspto-grants-2016_06 |
| ORD ID | ord-a07b86c049ee4927be9de9f79ad84b10 |
| Source note | uspto-grants-2016_06 |