HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 58486430, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-N-Boc-4-N-Methyl-aminopiperidine | HCID 2756806 | — |
| Reactant | 3,6-Dichloro-4,5-dimethylpyridazine | HCID 21187505 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58486430 | HCID 58486430 | 65% |
Reaction Steps
Heat a mixture of 3,6-dichloro-4,5-dimethylpyridazine (11.0 g, 62.1 mmol), tert-butyl methyl(piperidin-4-yl)carbamate (23.3 g, 109 mmol), and powdered K2CO3 (17.2 g, 124 mmol) in DMSO (310 mL) at 120° C. for 2 d. Cool the reaction mixture, dilute with H2O, and filter off the solid. Rinse the solid with H2O, and dry under vacuum at 45° C. Dissolve the solid in CH2Cl2, and pass the solution through a pad of silica gel, eluting with CH2Cl2. Concentrate the organic layer under reduced pressure to obtain the title compound as a yellow solid (14.3 g, 65%). ES/MS m/z (35Cl) 355.0 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08507490B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-0e280228bf874837b5fb25def8fb9b0b |
| Source note | uspto-grants-2013_08 |