反応 #2286381

反応方程式

2-bromo-4-methyl-thiazole-5-carboxylic acid ethyl ester

lithium hydroxide hydrate

hydrochloric acid

→

product

収率 98.0%

2-bromo-4-methyl-thiazole-5-carboxylic acid

収率 98.0%

溶媒

water

ethyl acetate

tetrahydrofuran

water

反応条件

後処理

1. 1
   抽出was extracted with ethyl acetate
2. 2
   乾燥The organic extracts were dried over sodium sulfate (Na2SO4)
3. 3
   ろ過filtered
4. 4
   濃縮concentrated

実験手順

To a solution of 2-bromo-4-methyl-thiazole-5-carboxylic acid ethyl ester (3.0 g, 12 mmol) in tetrahydrofuran (THF, 50 mL) and water (5 mL) was added lithium hydroxide hydrate (1.0 g, 24 mmol). The reaction mixture was stirred at ambient temperature for 16 h. The reaction mixture was diluted with water and ethyl acetate. The aqueous layer was made acidic to pH 1 with 2 N hydrochloric acid (HCl) and then was extracted with ethyl acetate. The organic extracts were dried over sodium sulfate (Na2SO4), filtered and concentrated to provide product as an orange solid (2.6 g, 98%): mp 152-155° C.; 1H NMR (300 MHz, CDCl3) δ 2.74 (s, 3H); ESIMS m/z 221 (M−1).

出典