反应详情

To a mixture of 0.041 g (0.089 mmole) of 2-[6-(4-methyl-piperazin-1-ylmethyl)-benzoimidazol-1-yl]-4-phenyl-thiazole-5-carboxylic acid ethyl ester (I.1a), 1 mL of tetrahydrofuran and 1 mL of water was added 0.011 g of lithium hydroxide. The reaction mixture was heated to 60 degrees for 30 minutes and then concentrated under reduced pressure. The mixture was diluted with 5 mL of water and then extracted with 5 mL of ethyl acetate. The pH of the aqueous layer was adjusted to ca 7 by addition of 1M hydrochloric acid and then extracted with 5 mL of ethyl acetate. A precipitate formed in aqueous layer after extraction. The solid was collected by filtration and air dried to give 0.025 g of 2-[6-(4-methyl-piperazin-1-ylmethyl)-benzoimidazol-1-yl]-4-phenyl-thiazole-5-carboxylic acid (I.1b) as an off-white solid.

1. temperatureThe reaction mixture was heated to 60 degrees for 30 minutes
2. concentrationconcentrated under reduced pressure
3. additionThe mixture was diluted with 5 mL of water
4. extractionextracted with 5 mL of ethyl acetate
5. additionby addition of 1M hydrochloric acid
6. extractionextracted with 5 mL of ethyl acetate
7. customA precipitate formed in aqueous layer
8. extractionafter extraction
9. filtrationThe solid was collected by filtration and air
10. customdried