تفاعل #7056

معادلة التفاعل

5-bromo-4-methylthiophene-2-sulfonamide

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title compound

المردود 43.0%

4-Methylthiophene-2-sulfonamide

المردود 43.0%

المذيبات

AcOH

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction mixture is heated
2. 2
   درجة الحرارةto reflux for 8 hr
3. 3
   درجة الحرارةthe reaction mixture is cooled
4. 4
   ترشيحfiltered
5. 5
   استخلاصThe aqueous layer is extracted with EtOAc (300 mL)
6. 6
   تجفيفThe organics are dried (Na2SO4)
7. 7
   ترشيحfiltered
8. 8
   تركيزconcentrated in vacuo
9. 9
   أخرىThe crude product is chromatographed on silica gel
10. 10
    غسيلeluting with CH2Cl2

الإجراء التجريبي

To a stirred solution of 5-bromo-4-methylthiophene-2-sulfonamide (3.1 g, 12.1 mmol) in AcOH (30 mL) is added zinc dust (2.4 g, 36.2 mmol). The reaction mixture is heated to reflux for 8 hr. After 8 hr, the reaction mixture is cooled and filtered. The filtrate is neutralized with 1 M NaOH. The aqueous layer is extracted with EtOAc (300 mL). The organics are dried (Na2SO4), filtered and concentrated in vacuo. The crude product is chromatographed on silica gel, eluting with CH2Cl2 to afford the title compound (0.90 g, 43%).

المصدر