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N,N-Diethyl-1,4-butanediamine → 1-Cyclopropyl-7-(4-diethylamino-butylamino)-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-Diethyl-1,4-butanediamine | HCID 117976 | — |
| 反応物 | 1-cyclopropyl-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-7-methanesulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one | HCID 18444694 | — |
| 反応物 | EtOH ethyl acetate triethylamine | HCID 22328969 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 1-Cyclopropyl-7-(4-diethylamino-butylamino)-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one | HCID 10323850 | 83% |
反応手順
Using Procedure K, 0.63 g (1.48 mmol) of 1-cyclopropyl-3-(2,6-difluoro-3,5-dimethoxy-phenyl)-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 0.62 g (83%) of the title compound as a solid: mp 139° C.–141° C. MS (APCI) (m+1)/z 505.2. Analysis calculated for C25H34N6F2O3: C, 59.51; H, 6.79; N, 16.66. Found: C, 59.56; H, 6.77; N, 16.49.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07196090B2 |
| 出典データセット | uspto-grants-2007_03 |
| ORD ID | ord-ad02a537a6d64c6a8d1abf44a0cc9f76 |
| 出典メモ | uspto-grants-2007_03 |