반응 #359818

반응 방정식

Prop-2-yn-1-ol

2,4-Dichloro-5-trifluoromethyl-pyrimidine

Trifluoro-acetic acid

→

2-Chloro-4-prop-2-ynyloxy-5-trifluoromethyl-pyrimidine

반응 조건

후처리

1. 1
   workup.ADDITIONThe batch is poured on ice
2. 2
   추출extracted with ethyl acetate (3×)
3. 3
   세척The combined organic phases are washed with water
4. 4
   건조dried (Na2SO4)
5. 5
   여과filtered
6. 6
   농축concentrated by evaporation
7. 7
   기타The remaining residue is purified by chromatography (hexane/ethyl acetate 95:5)
8. 8
   기타591 mg (2.5 mmol, corresponding to 16% of theory) of the product is obtained

실험 절차

3.97 ml (68.2 mmol) Prop-2-yn-1-ol are slowly added to 3.40 g (15.6 mmol) of 2,4-Dichloro-5-trifluoromethyl-pyrimidine at 0° C. under a nitrogen atmosphere. 0.79 ml Trifluoro-acetic acid are added dropwise and the batch is stirred for 6 hours at 0° C. The batch is poured on ice and extracted with ethyl acetate (3×). The combined organic phases are washed with water, dried (Na2SO4), filtered and concentrated by evaporation. The remaining residue is purified by chromatography (hexane/ethyl acetate 95:5). 591 mg (2.5 mmol, corresponding to 16% of theory) of the product is obtained.

출처