반응 #558593

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 solvent is removed under reduced pressure
2. 2
   workup.ADDITIONAqueous 1 M HCl is added until pH 5
3. 3
   여과The precipitated product is filtered off
4. 4
   세척washed with ACN
5. 5
   건조After drying 1.3 g (32%) of the desired product
6. 6
   기타are obtained a solid material

실험 절차

The title compound is synthesized according to general procedure GP8 starting from 4.0 g (10.3 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 solvent is removed under reduced pressure and the residue is taken up in water. Aqueous 1 M HCl is added until pH 5 is reached. The precipitated product is filtered off and washed with ACN. After drying 1.3 g (32%) of the desired product are obtained a solid material.

출처