반응 #10497

반응 방정식

7-Bromo-3-hydroxy-4H-benzo[1,4]thiazine-2-carboxylic acid ethyl ester

→

(6-bromo-benzothiazol-2-yl)-acetic acid ethyl ester

용매

acetic acid

반응 조건

후처리

1. 1
   온도cooled to room temperature
2. 2
   여과Zinc was filtered off
3. 3
   세척rinsed with 20 mL EtOAc
4. 4
   농축The combined filtrate was concentrated to yellow crystals
5. 5
   기타purified by column chromatography (silica gel, 20:90 EtOAc:hexane)

실험 절차

7-Bromo-3-hydroxy-4H-benzo[1,4]thiazine-2-carboxylic acid ethyl ester (2.47 g, 7.8 mmol) was dissolved in 50 mL of acetic acid and heated to 110° C. under nitrogen. Zinc powder (7.5 g, 114.7 mmol) was added in portions at room temperature over 80 minutes. The mixture was stirred at 110° C. for additional 2 hours and cooled to room temperature. Zinc was filtered off and rinsed with 20 mL EtOAc. The combined filtrate was concentrated to yellow crystals and purified by column chromatography (silica gel, 20:90 EtOAc:hexane) to give (6-bromo-benzothiazol-2-yl)-acetic acid ethyl ester.

출처