반응 #558604

반응 방정식

4-[5-(6-amino-2-methyl-pyridin-3-ylethynyl)-6-ethyl-pyrimidin-4-yl]-2-fluoro-benzoic acid methyl ester

LiOH

→

title compound

4-[5-(6-Amino-2-methyl-pyridin-3-ylethynyl)-6-ethyl-pyrimidin-4-yl]-2-fluoro-benzoic acid

용매

THF

water

반응 조건

후처리

1. 1
   기타The THF is removed under reduced pressure
2. 2
   workup.ADDITIONAqueous 1 M HCl is added until pH 5-6
3. 3
   여과The precipitated product is filtered off
4. 4
   세척washed with water and MeOH
5. 5
   건조After drying 1.25 g (32%) of the desired product
6. 6
   기타is obtained a solid material

실험 절차

The title compound is synthesized according to general procedure GP8 starting from 4.0 g (10.2 mmol) 4-[5-(6-amino-2-methyl-pyridin-3-ylethynyl)-6-ethyl-pyrimidin-4-yl]-2-fluoro-benzoic acid methyl ester using 1.29 g (30.7 mmoL) LiOH in 40 mL water and 200 mL THF. The reaction mixture is stirred over night at 50° C. The THF is removed under reduced pressure and the residue is taken up in water. Aqueous 1 M HCl is added until pH 5-6 is reached. The precipitated product is filtered off and washed with water and MeOH. After drying 1.25 g (32%) of the desired product is obtained a solid material.

출처