反応式
[NH2:1][C:2]1[N:7]=[C:6](OS(C(F)(F)F)(=O)=O)[C:5]([CH3:16])=[C:4]([C:17]2[O:18][CH:19]=[CH:20][CH:21]=2)[N:3]=1.[CH2:22]([NH2:29])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.O>COCCOC>[CH2:22]([NH:29][C:6]1[C:5]([CH3:16])=[C:4]([C:17]2[O:18][CH:19]=[CH:20][CH:21]=2)[N:3]=[C:2]([NH2:1])[N:7]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1参加物
5
反応条件
- 温度
- 80 °C
実験手順
To a stirred solution of 250 mg (0.77 mmol) trifluoromethanesulfonic acid 2-amino-6-furan-2-yl-5-methyl-pyrimidin-4-yl ester in 10 ml DME in a pressure tube was added 0.63 ml (5.77 mmol) benzylamine and the mixture heated at 80° C. for 16 hours. The reaction mixture was then poured onto 80 ml water and cooled to 0° C. The resulting crystals were collected by filtration and washed sequentially with water, ether/hexane and a minimum quantity of ice-cold ether to afford 140 mg (65%) N4-benzyl-6-furan-2-yl-5-methyl-pyrimidine-2,4-diamine as a white crystalline solid. ES-MS m/e (%): 281 (M+H+, 100).
後処理
- temperaturecooled to 0° C
- filtrationThe resulting crystals were collected by filtration
- washwashed sequentially with water, ether/hexane
出典と根拠
- ORDレコード
- ord-26c9deab248d49f58df10f9835e7cfac
- 出典データセット
- uspto-grants-2003_07
- 特許番号
- US06586441B2
関連ノート
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