HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dimethoxyethane → HCID 54519761, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dimethoxyethane | HCID 8071 | — |
| Reactant | HCID 53672099 | HCID 53672099 | — |
| Catalyst | ruthenium;triphenylphosphane | HCID 11981970 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 54519761 | HCID 54519761 | — |
Reaction Steps
A mixture of 5-amino-1-tert-butyl-4-cyano-3-(4-methoxycarbonylphenyl)pyrazole (448 mg, 1.5 mmol) and tetrakis(triphenylphosphine)ruthenium dihydride in dimethoxyethane (1 ml) and water (54 μl) was heated at 120° under a nitrogen atmosphere in a sealed tube for 18 h. The reaction was concentrated under reduced pressure and the residue subjected to column chromatography (silica 4% methanol-CH2Cl2) to give the title compound (170 mg) after recrystallisation from ethyl acetate as a colourless solid m.p. 237-239°. δH (CDCl3) 1.67 (9H, s), 4.39 (3H, s), 5.10 (2H, br s), 5.69 (2H, br s), 7.66 (2H, d, J 8.2 Hz), and 8.11 (2H, d, J 8.3 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05922741 |
| Source dataset | uspto-grants-1999_07 |
| ORD ID | ord-7c9d6fa57e444aafbe9f6c23ef780be8 |
| Source note | uspto-grants-1999_07 |