反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1.[H-].[Na+].Cl[C:15]1[CH:20]=[C:19]([C:21]([F:24])([F:23])[F:22])[N:18]=[C:17]([S:25][CH3:26])[N:16]=1>C1COCC1>[CH3:26][S:25][C:17]1[N:18]=[C:19]([C:21]([F:24])([F:22])[F:23])[CH:20]=[C:15]([O:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:10])([F:11])[F:1])[CH:4]=2)[N:16]=1参加物
5
実験手順
m-(Trifluoromethyl)phenol (1.06 g, 0.0044×1.5 mol) and NaH (0.26 g (ca.60% in mineral oil), 0.0044×1.5 mol) were dissolved in THF, and then 4-chloro-2-methylthio-6-(trifluoromethyl)pyrimidine (Compound No. VII-17) (1.0 g, 0.0044 mol) was added thereto. The resulting solution was refluxed for about 7 hours. The reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate to separate an organic phase. The organic phase was washed with aqueous saturated sodium chloride, dried over anhydrous sodium sulfate and concentrated. Thereafter, remaining phenol and others were distilled off in a tubular oven (under water flow, 150° C.) to obtain the intermediate compound.
後処理
- additionVII-17) (1.0 g, 0.0044 mol) was added
- temperatureThe resulting solution was refluxed for about 7 hours
- customThe reaction solution was partitioned between ethyl acetate and aqueous saturated sodium hydrogen carbonate
- customto separate an organic phase
- washThe organic phase was washed with aqueous saturated sodium chloride
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- distillationwere distilled off in a tubular oven (under water flow, 150° C.)
- customto obtain the intermediate compound
出典と根拠
- ORDレコード
- ord-779700042b074f55b42f3a2202e7c555
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05723412
関連ノート
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