HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butyl nitrite → HCID 21188047, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | HCID 22618399 | HCID 22618399 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21188047 | HCID 21188047 | — |
Reaction Steps
To a stirred solution of 5-amino -1-(2,6-dichloro-4-trifluoromethylphenyl)-4-iodo-3-methylpyrazole (2.85 g) in tetrahydrofuran (35 ml) at 0° C. was added dropwise t-butylnitrite (2.33 ml). The reaction mixture was allowed to warm to room temperature and then heated under reflux for 1.5 hours. The reaction mixture was evaporated and the residue purified by column chromatography on silica gel eluted with dichloromethane: hexane (1:1). Combination and evaporation of suitable fractions provided a yellow oil which was further purified by column chromatography on silica gel eluted with dichloromethane: hexane (1:2). Combination and evaporation of suitable fractions provided the title compound as a white solid, m.p. 118.5-119.4° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06255333B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-35481554bfab4dd084d5c5387154cba8 |
| Source note | uspto-grants-2001_07 |