HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 67112048, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 67112246 | HCID 67112246 | — |
| Reactant | HCID 86666562 | HCID 86666562 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67112048 | HCID 67112048 | 140.7% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
Add 5-chloro-3-(2,2,2-trifluoroethyl)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one (0.28 g, 1.05 mmol), 2-(4-ethyl-2-(piperidin-4-yl)-1H-imidazol-1-yl)ethanol dihydrochloride (0.38 g, 1.3 eq), methanol (15 mL) and diisopropylethylamine (0.91 mL, 5.0 eq) into a 20 mL microwave vial. Seal the tube and heat in a microwave reactor to 150° C., for 1 hour. Filter through silica gel, eluting with 10% ammonia-methanol/dichloromethane. Concentrate the filtrate in vacuo. Purify by silica gel chromatography, eluting with 3:1 ethyl acetate/methanol, to give the title compound as a yellow foam (0.67 g, 70%). MS (ES) m/z=454 [M]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08436002B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-2b73a62f4b814a35804ad8220cdf793f |
| Source note | uspto-grants-2013_05 |