4-Hydroxy-6-(trifluoromethyl)pyrimidine synthesis
- Product Name:4-Hydroxy-6-(trifluoromethyl)pyrimidine
- CAS Number:1546-78-7
- Molecular formula:C5H3F3N2O
- Molecular Weight:164.09
Yield: 96%
Reaction Conditions:
with 1,8-diazabicyclo[5.4.0]undec-7-ene in ethanol at 70 - 80;
Steps:
2 (2) Synthesis of 4-hydroxy-6-trifluoromethylpyrimidine
To a three-necked flask was added ethyl trifluoroacetoacetate (0.16 mL, 1.0 eq.),DBU (0.19 mL, 1.2 eq.),Add absolute ethanol (10 mL) to dissolve.A solution of formamidine hydrochloride in ethanol (0.09 g of formamidine hydrochloride in 2 mL of ethanol,The amount of formamidine hydrochloride1.05 eq.).Dropping the temperature to 70-80 ° C for 3 to 5 hours.TLC monitoring,The reaction was complete.The solvent was distilled off under reduced pressure,Diluted with water (20 mL)With 1mol / L hydrochloric acid adjusted pH = 6 ~ 7,Extraction with ethyl acetate (3 x 8 mL)The organic phase was combined with anhydrous sulfuric acidSodium drying, filtration, vacuum distillation of the solvent was light yellow solid, add petroleum ether (5mL) shock, filter, filter cake washed with petroleum ether,The oven was dried at 55 ° C for 2 hours to give a pale yellow flake solid in 96% yield.
References:
China Pharmaceutical University;Dai, Zhenya;Xu, Pei;Yu, Qiuhan;Zhao, Yunde CN106188013, 2016, A Location in patent:Paragraph 0012; 0013; 0019
6313-33-3
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