반응 #2468008
ord-bbe8789f04bc4773a5970af04c4b6545
반응 방정식
2,4-dichloro-5-methoxy-pyrimidine
4,5,6,7-tetrahydroimidazopyridine dihydrochloride
ethyldiisopropylamine
→
2-chloro-4-(3,4,6,7-tetrahydro-imidazo[4,5-c]pyridin-5-yl)-5-methoxy-pyrimidine
반응물
시약
없음
용매
반응 조건
온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타The crude mixture is purified by column chromatography
- 2workup.ADDITION0.2% formic acid is added to both eluants
- 3기타The suitable fractions are freeze-dried
실험 절차
1 g 2,4-dichloro-5-methoxy-pyrimidine are dissolved in 4 mL butanol and combined with 1.04 g 4,5,6,7-tetrahydroimidazopyridine dihydrochloride and 2.96 mL ethyldiisopropylamine. This mixture is stirred for 16 h at 50° C. and then the solvent is eliminated in vacuo. The crude mixture is purified by column chromatography. The carrier material used is C18-RP-silica gel and a gradient is run through which consists at the starting point of 95% water and 5% acetonitrile and at the finishing point of 70% water and 30% acetonitrile. 0.2% formic acid is added to both eluants. The suitable fractions are freeze-dried.