反応式
P(Cl)(Cl)(Cl)=O.[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[NH:14][C:15](=O)[CH:16]=[C:17]([C:19]([OH:21])=[O:20])[N:18]=2)=[CH:9][CH:8]=1.C(#[N:25])C>O>[NH2:25][C:15]1[N:14]=[C:13]([C:10]2[CH:11]=[CH:12][C:7]([Cl:6])=[CH:8][CH:9]=2)[N:18]=[C:17]([C:19]([OH:21])=[O:20])[CH:16]=1参加物
反応条件
- 温度
- 90 °C
実験手順
To phosphorus oxychloride (180 mL) was added 2-(4-chlorophenyl)-1,6-dihydro-6-oxo-4-pyrimidinecarboxylic acid (i.e. the product of Step A) (81.81 g, 326 mmol). The mixture was heated to 90° C. for 2.5 h. After cooling to room temperature the reaction mixture was slowly added to 1:2 acetonitrile:water (1.5 L) while keeping the temperature between 35 and 45° C. After the reaction mixture was stirred at room temperature for 30 minutes the resulting solid was isolated by filtration and washed with water. The solid was then combined with aqueous ammonia (5%, 2.1 L) and heated to 80° C. for 18 h. After 2 days at room temperature the solid was isolated by filtration and washed with water. A second crop was obtained by cooling the filtrate and refiltering. The combined solids were dried to afford the title compound (58.8 g).
後処理
- temperatureAfter cooling to room temperature the reaction mixture
- customthe temperature between 35 and 45° C
- customwas isolated by filtration
- washwashed with water
- temperatureheated to 80° C. for 18 h
- customAfter 2 days at room temperature the solid was isolated by filtration
- washwashed with water
- customA second crop was obtained
- temperatureby cooling the filtrate and refiltering
- customThe combined solids were dried
出典と根拠
- ORDレコード
- ord-3eefd357afef4416b790c105dabe9d0e
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09144240B2
関連ノート
読み込み中…