HuagongsheHuagongshe Chemistry Print Report · For research reference only
N,N-Diethyl-1,4-butanediamine → 1-Cyclopentyl-7-(4-diethylamino-butylamino)-3-(3-ethoxy-2,6-difluoro-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N,N-Diethyl-1,4-butanediamine | HCID 117976 | — |
| Reactant | 3-(3-ethoxy-2,6-difluoro-phenyl)-1-(1-ethyl-propyl)-7-methanesulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one | HCID 18444795 | — |
| Reactant | EtOH ethyl acetate triethylamine | HCID 22328969 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 1-Cyclopentyl-7-(4-diethylamino-butylamino)-3-(3-ethoxy-2,6-difluoro-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one | HCID 10075251 | 86% |
Reaction Steps
Using Procedure K, described above, 0.74 g (1.69 mmol) of 3-(3-ethoxy-2,6-difluoro-phenyl)-1-(1-ethyl-propyl)-7-methanesulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one and 4-(diethylamino)butylamine in 20 mL of dioxane were reacted. Chromatography with 9:1:0.5 ethyl acetate/ethanol/ triethylamine gave 0.75 g (86%) of the title compound as a solid: mp 129° C.–130° C. 130° C. MS (APCI) (m+1)/z 5127.47. Analysis calculated for C27H38N6F2O2: C, 62.77; H, 7.41; N, 16.27.Found: C, 62.79; H, 7.35; N, 16.10.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07196090B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-d5e9e47280464c72b78f3c7713768875 |
| Source note | uspto-grants-2007_03 |