تفاعل #10497

معادلة التفاعل

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

→

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

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled to room temperature
2. 2
   ترشيحZinc was filtered off
3. 3
   غسيلrinsed with 20 mL EtOAc
4. 4
   تركيزThe combined filtrate was concentrated to yellow crystals
5. 5
   أخرىpurified by column chromatography (silica gel, 20:90 EtOAc:hexane)

الإجراء التجريبي

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.

المصدر