تفاعل #1058371

معادلة التفاعل

water

N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

2,3-dichloropyridine

N,N-diisopropylethylamine

→

white solid

المردود 57.4%

7-(3-Chloropyridin-2-yl)-N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine

المردود 57.4%

المذيبات

1,4-dioxane

N,N-dimethylacetamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto cool to room temperature
2. 2
   استخلاصThe mixture was extracted with ethyl acetate (2×30 mL)
3. 3
   غسيلthe combined organic layers were washed with brine
4. 4
   تجفيفdried over sodium sulfate
5. 5
   تركيزconcentrated
6. 6
   أخرىto leave an oil
7. 7
   أخرىThe residue was purified by flash chromatography over silica gel (ethyl acetate/hexane gradient 0 to 100%)

الإجراء التجريبي

A mixture of N-(4-(trifluoromethyl)phenyl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4-amine (0.250 g, 0.85 mmol), 2,3-dichloropyridine (0.251 g, 1.69 mmol) and N,N-diisopropylethylamine (0.22 mL, 1.27 mmol) in a mixture of 1,4-dioxane (2 mL) and N,N-dimethylacetamide (0.2 mL) was heated in a sealed tube via microwave (Emerys Optimizer model, Personal Chemistry) for 10 hr at 170° C. The mixture was allowed to cool to room temperature and poured into water (60 mL). The mixture was extracted with ethyl acetate (2×30 mL) and the combined organic layers were washed with brine, dried over sodium sulfate and concentrated to leave an oil. The residue was purified by flash chromatography over silica gel (ethyl acetate/hexane gradient 0 to 100%) to obtain 198 mg of a white solid.

المصدر