三氟乙脒 → 2,4-二三氟甲基-5-嘧啶甲酸乙酯
反应方程式
C(O[CH:4]=[C:5]([C:11]([C:13]([F:16])([F:15])[F:14])=O)[C:6]([O:8][CH2:9][CH3:10])=[O:7])C.[F:17][C:18]([F:23])([F:22])[C:19]([NH2:21])=[NH:20]>CCO>[CH2:9]([O:8][C:6]([C:5]1[C:11]([C:13]([F:14])([F:15])[F:16])=[N:20][C:19]([C:18]([F:23])([F:22])[F:17])=[N:21][CH:4]=1)=[O:7])[CH3:10]参与物
4
实验过程
A solution of ethyl ethoxymethylene-4,4,4-trifluoroacetoacetate (15 g, 62.5 mmol) and trifluoroacetamidine (12.6 g, 112.5 mmol) in EtOH (50 mL) was heated at reflux for 24 h under N2. The reaction mixture was cooled and concentrated. Chromatography (SiO2, 20% EtOAc/hexane) afforded ethyl-2,4-bis (trifluoromethyl)pyrimidine-5-carboxylate as an oil (7.0 g, 39%), 1HNMR (CDCl3) δ 9.37 (s, 1H), 3.70 (q, 2H), 1.27 (t, 3H).
后处理
- temperatureat reflux for 24 h under N2
- temperatureThe reaction mixture was cooled
- concentrationconcentrated
来源与证据
- ORD记录
- ord-4baead46329c48d7a417b6270e76d3e4
- 来源数据集
- uspto-grants-1998_09
- 专利号
- US05811428
反应笔记
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