HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butyl nitrite → HCID 21188102, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | HCID 21188050 | HCID 21188050 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21188102 | HCID 21188102 | — |
Reaction Steps
To a stirred solution of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-methyl 4-trimethylsilylethynylpyrazole (1.3 g) in tetrahydrofuran (15 ml) at 65° C. was added dropwise t-butylnitrite (1.65 g) in tetrahydrofuran (5 ml) over a period of 15 minutes and heating continued for 3 hours. The reaction mixture was left at room temperature overnight then evaporated to give the crude product as a gum which was purified by column chromatography on silica gel eluted with dichioromethane:hexane (1:1). Combination and evaporation of appropriate fractions provided the title compound as a pale yellow solid, m.p. 76-78° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06255333B1 |
| Source dataset | uspto-grants-2001_07 |
| ORD ID | ord-184e85656ae94fadb83ca3865a98e043 |
| Source note | uspto-grants-2001_07 |