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Water → 6-(2,6-Dichlorophenyl)-N2-phenyl-pyrido[2,3-d]-pyrimidine-2,7-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | (2,6-Dichlorophenyl)acetonitrile | HCID 76678 | — |
| 反応物 | 4-Amino-2-phenylamino-pyrimidine-5-carboxaldehyde | HCID 18375311 | — |
| 溶媒 | Glycol monoethyl ether | HCID 8076 | — |
| 生成物 | 6-(2,6-Dichlorophenyl)-N2-phenyl-pyrido[2,3-d]-pyrimidine-2,7-diamine | HCID 70285163 | 68.4% |
反応手順
To a solution of 0.022 g 60% sodium hydride suspension in 2.00 mL of 2-ethoxyethanol was added 0.46 g of 2,6-dichlorophenylacetonitrile and 0.50 g of 4-amino-2-phenylamino-pyrimidine-5-carboxaldehyde from Example 72. The reaction was refluxed for 4 hours, cooled, poured into water, and extracted several times with dichloromethane. The dichloromethane washes were combined, washed with saturated sodium chloride, dried with magnesium sulfate, and concentrated in vacuo. The residue was washed with diethyl ether to give 0.61 g of the title compound, CIMS (1% NH3 in CH4): 410=M+ +C2H5, 382=M+ +H, 381=M+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733913 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-32214df9473647ba998abcb895c010fa |
| 出典メモ | uspto-grants-1998_03 |