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Dimethylformamide dimethyl acetal → N'-[6-(2,6-dichlorophenyl)-7-[(dimethylamino)-methyleneamino]-pyrido[2,3-d]pyrimidin-2-yl]-N,N-dimethylformamidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 反応物 | 6-(2,6-Dichlorophenyl)pyrido[2,3-d]pyrimidine-2,7-diamine | HCID 5328113 | — |
| 生成物 | N'-[6-(2,6-dichlorophenyl)-7-[(dimethylamino)-methyleneamino]-pyrido[2,3-d]pyrimidin-2-yl]-N,N-dimethylformamidine | HCID 54482161 | — |
反応手順
2,7-Diamino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]-pyrimidine from Example 1 was reacted with DMF dimethyl acetal for 23 hours as described in Example 78. Workup as described above followed by purification on flash silica gel chromatography eluting sequentially with 100:0, 9:1, 4:1, and 7:3 ethyl acetate:methanol gave an oil that was crystallized from ethyl acetate to afford N'-[6-(2,6-dichlorophenyl)-7-[(dimethylamino)-methyleneamino]-pyrido[2,3-d]pyrimidin-2-yl]-N,N-dimethylformamidine, mp 269-272° C. CIMS (1% ammonia in methane): m/z (relative intensity) 418 (MH+ +2, 60), 416 (MH+, 100).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05952342 |
| 出典データセット | uspto-grants-1999_09 |
| ORD ID | ord-7ecf1d3e4c724238b8bcc75bf61f08e8 |
| 出典メモ | uspto-grants-1999_09 |