反应详情

To a mixture of 0.066 g of 2-[5-(4-methyl-piperazin-1-ylmethyl)-2-nitro-phenylamino]-4-phenyl-thiazole-5-carboxylic acid ethyl ester (VI.1c), 0.5 mL of 1M hydrochloric acid, 2 mL of tetrahydrofuran was added 0.060 g of zinc powder. The suspension was stirred at ambient temperature for 2 hours. The solid was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was diluted with 2 mL of saturated sodium bicarbonate, 10 mL of water and extracted three times with 5 mL of dichloromethane. The combined organic layers were washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to give 2-[2-amino-5-(4-methyl-piperazin-1-ylmethyl)-phenylamino]-4-phenyl-thiazole-5-carboxylic acid ethyl ester (VII.1a) as a yellow oil. This material was carried to next step of reaction without further purification.

1. customThe solid was removed by filtration
2. concentrationthe filtrate was concentrated under reduced pressure
3. additionThe residue was diluted with 2 mL of saturated sodium bicarbonate, 10 mL of water
4. extractionextracted three times with 5 mL of dichloromethane
5. washThe combined organic layers were washed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure