تفاعل #40420

معادلة التفاعل

5-chloroisatoic anhydride

2-amino-5-chloropyridine

potassium bis(trimethylsilyl)amide

toluene

→

(2-amino-5-chlorophenyl)-N-(5-chloro(2-pyridyl))carboxamide

المردود 99.0%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe mixture was warmed up
2. 2
   workup.STIRRINGstirred overnight
3. 3
   تركيزAfter concentrated
4. 4
   غسيلthe crude was washed with saturated ammonium chloride solution
5. 5
   استخلاصextracted by ethyl acetate
6. 6
   تجفيفThe organic layer was dried over magnesium sulfate
7. 7
   تركيزconcentrated

الإجراء التجريبي

To a solution of 2-amino-5-chloropyridine (787 mg, 6.1 mmol) in tetrahydrofuran (5 ml) was added 0.5M potassium bis(trimethylsilyl)amide in toluene (20 ml, 10.1 mmol) dropwise at −78° C. After stirred for additional 0.5 hr at −78° C., the mixture was added 5-chloroisatoic anhydride (1 g, 5.1 mmol) at −78° C. The mixture was warmed up to r.t gradually and stirred overnight. After concentrated, the crude was washed with saturated ammonium chloride solution and extracted by ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated to give (2-amino-5-chlorophenyl)-N-(5-chloro(2-pyridyl))carboxamide as yellow solid (1.39 g, 99%). MS found for C12H9Cl2N3O M+=282, (M+2)+=284.

المصدر