HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86753306, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | 3-Methyl-2-butanone | HCID 11251 | — |
| Reactant | HCID 18940147 | HCID 18940147 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86753306 | HCID 86753306 | — |
Reaction Steps
A solution of 1-[4,6-bis[trifluoromethyl]pyrid-2-yl]-1-methyl hydrazine (40.04 g; 0.15 mol), 3-methyl-2-butanone (14.2 g; 0.165 mol) and p-toluenesulphonic acid (0.32 g) in toluene (90 ml) was heated under reflux, with water removal (azeotrope), for 40 h. The solution was concentrated to yield a dark oil which was purified by flash-chromatography over silica (eluent: petroleum ether 60/80) to yield 3-methyl-2-butanone 1-[4,6-bis[trifluoromethyl]pyrid-2-yl]-1-methyl hydrazone as a red oil (10.9 g; 22%). ##STR26##
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05833885 |
| Source dataset | uspto-grants-1998_11 |
| ORD ID | ord-7e1a11bccaf84722a0c11efffd338509 |
| Source note | uspto-grants-1998_11 |