反応式
CS([C:5]1[N:10]=[C:9]([C:11]2[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:13][CH:12]=2)[CH:8]=[C:7]([C:21]([F:24])([F:23])[F:22])[N:6]=1)(=O)=O.[CH:25]1([NH2:30])[CH2:29][CH2:28][CH2:27][CH2:26]1>CC#N>[CH:25]1([NH:30][C:5]2[N:10]=[C:9]([C:11]3[CH:16]=[CH:15][C:14]([S:17]([CH3:20])(=[O:19])=[O:18])=[CH:13][CH:12]=3)[CH:8]=[C:7]([C:21]([F:24])([F:23])[F:22])[N:6]=2)[CH2:29][CH2:28][CH2:27][CH2:26]1参加物
4
実験手順
To a stirred solution of 2-(methylsulfonyl)-4-[4-(methylsulfonyl)phenyl]-6-(trifluoromethyl)pyrimidine (0.50 g, 1.31 mmol) in MeCN (10 ml) was added cyclopentylamine (0.34 g) and the resultant solution heated under reflux for 18 h. The cooled reaction mixture was concentrated in vacuo and the residue partitioned between 2N HCl and ethyl acetate. The organic phase was separated, washed with 2N HCl then water and concentrated in vacuo to a yellow oil. This oil was purified by SPE chromatography with cyclohexane:ethyl acetate (3:1) as eluant. Concentration in vacuo of the combined fractions containing pure product gave crystals which were isolated by filtration to give the title compound as a white crystalline solid (0.21 g, 53%).
後処理
- temperatureunder reflux for 18 h
- customThe cooled reaction mixture
- concentrationwas concentrated in vacuo
- customthe residue partitioned between 2N HCl and ethyl acetate
- customThe organic phase was separated
- washwashed with 2N HCl
- concentrationwater and concentrated in vacuo to a yellow oil
- customThis oil was purified by SPE chromatography with cyclohexane:ethyl acetate (3:1) as eluant
- concentrationConcentration in vacuo of the combined fractions
- additioncontaining pure product
- customgave crystals which
- customwere isolated by filtration
出典と根拠
- ORDレコード
- ord-11f08ec5f5df49d4b11758e1014454fe
- 出典データセット
- uspto-grants-2004_08
- 特許番号
- US06780869B1
関連ノート
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