HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 53353686, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 53353683 | HCID 53353683 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 53353686 | HCID 53353686 | — |
Reaction Steps
4-Chloro-5-methylamino-2-(3,3,5,5-tetramethylcyclohexyl)pyridazin-3-one (0.15 g, 0.5 mmoles) was dissolved in ethanol (20 mL) and 1M sodium hydroxide (1 ml) was added. 10% Palladium on charcoal (40 mg) was added and the reaction mixture was stirred overnight under a balloon of hydrogen. Filtered off the catalyst and evaporated to a low bulk. Partitioned between water and ethyl acetate, separated and dried over magnesium sulphate. Evaporated to give the required product as a buff solid. (0.125 g, 94%). 1H NMR (300 MHz CDCl3) 7.32 (d, 1H, J=3 Hz), 5.7 (d, 1H, J=3 Hz), 5.3 (m, 1H), 4.2 (brs, 1H), 2.85 (d, 3H, J=5 Hz), 1.55 (m, 4H), 1.3 (m, 1H), 1.15 (m, 1H), 1.15 (s, 6H), 0.95 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062004B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-4bb4ca08512a4345a03e2d4c69c9807c |
| Source note | uspto-grants-2015_06 |