تفاعل #2324990

معادلة التفاعل

2-Chloro-4-methyl-thiazole

thionyl chloride

chlorosulfonic acid

→

2-Chloro-4-methyl-thiazole-5-sulfonyl chloride

المردود 43.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةcooled
2. 2
   workup.ADDITIONthen poured onto ice-water
3. 3
   استخلاصextracted 3 times with CH2Cl2
4. 4
   تجفيفdried over Na2SO4
5. 5
   ترشيحfiltered
6. 6
   تركيزconcentrated
7. 7
   أخرىto give a crude liquid
8. 8
   أخرىThe product was isolated by simple distillation (17 mbar at 85-95° C.)

الإجراء التجريبي

2-Chloro-4-methyl-thiazole (33 g, 180 mmol) was added dropwise to a solution of thionyl chloride (32.7 mL, 451 mmol) and chlorosulfonic acid (60.2 mL, 902 mmol). The reaction mixture was stirred for 48 h at 120° C., cooled then poured onto ice-water and extracted 3 times with CH2Cl2, dried over Na2SO4, filtered, and concentrated to give a crude liquid. The product was isolated by simple distillation (17 mbar at 85-95° C.) to give 2-Chloro-4-methyl-thiazole-5-sulfonyl chloride (17.85 g, 43%) as a light-yellow liquid. MS (ISP) 233.0[(M+H)+].

المصدر