Diisopropylethylamine → 2-chloro-N-methyl-5-nitropyrimidin-4-amine
反応式
CN.C(O)C.[CH:6]([N:9](CC)C(C)C)(C)C.[Cl:15][C:16]1[N:21]=[C:20](Cl)[C:19]([N+:23]([O-:25])=[O:24])=[CH:18][N:17]=1>ClCCl>[Cl:15][C:16]1[N:21]=[C:20]([NH:9][CH3:6])[C:19]([N+:23]([O-:25])=[O:24])=[CH:18][N:17]=1参加物
5
実験手順
A solution of methyl amine-ethanol (7.6 ml) and N,N-diisopropylethylamine (13.2 ml) were dissolved into 150 ml dichloromethane. The mixture was added dropwise to a solution of 2,4-dichloro-5-nitropyrimidine (10.0 g) in dichloromethane (30 ml) at 0° C. After the completion of the dropwise addition, the mixture was kept at the same temperature to react for half an hour. Purification was conducted by a column chromatography to obtain a yellow solid (8.3 g) in a yield of 85.4%. 1H NMR (400 MHz, CDCl3): δ 9.05 (s, 1H), 8.41 (s, 1H), 3.22 (s, 3H) ppm.
後処理
- additionAfter the completion of the dropwise addition
- customto react for half an hour
- customPurification
出典と根拠
- ORDレコード
- ord-075d87a7989c43cca1cf80dc2d258182
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09096601B2
反応ノート
読み込み中…