HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 74344756, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Hexane | HCID 8058 | — |
| Reactant | HCID 69314056 | HCID 69314056 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 74344756 | HCID 74344756 | 86% |
Reaction Steps
To a solution of dimethylamine (0.051 mL, 1 mmol) in DCE was added a solution of TMA 2M in hexane (499 mmol, 1 mmol) and the mixture was stirred 30 min at r.t. To this solution was added a solution of methyl N-{4-[(4-tert-butyl-1,3-thiazol-2(3H)-ylidene)(cyano)methyl]pyrimidin-2-yl}-beta-alaninate (72 mg, 0.2 mmol) in DCE and the mixture was refluxed under inert atmosphere overnight then stirred for a week at r.t. The mixture was diluted with DCM then water was added. The suspension was filtered through celite. The filtrate was washed with aqueous NaHCO3 5% (×2) then brine and it was dried over MgSO4. The solvent was removed under reduced pressure affording the title compound as yellow solid (HPLC max plot 86%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07465736B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-2aea5c96da35404b9d473582a381560e |
| Source note | uspto-grants-2008_12 |