Реакция #40476

Уравнение реакции

di-HCl

2-methyl nicotinic acid

6-chloro-7-fluoro-9H-β-carbolin-8-ylamine

EDCI

→

N-(6-chloro-7-fluoro-9H-β-carbolin-8-yl)-2-methyl-nicotinamide

Растворители

pyridine

Условия реакции

Обработка

1. 1
   ДругоеThe pyridine was removed under reduced pressure
2. 2
   Другоеthe resulting dark oil was triturated with saturated aqueous NaHCO3
3. 3
   ДругоеThe precipitate which formed
4. 4
   Фильтрацияwas filtered
5. 5
   Промывкаwashed with MeOH
6. 6
   workup.ADDITIONThe material was treated with 2M HCl in Et2O
7. 7
   Другоеto yield a gray solid

Методика

A solution of 6-chloro-7-fluoro-9H-β-carbolin-8-ylamine (100 mg, 0.424 mmol) in pyridine (2.5 ml) was stirred at RT. 2-methyl nicotinic acid (70 mg, 0.509 mmol) was added, followed by EDCI (130 mg, 0.678 mmol). The suspension was stirred at 100° C. for a day. The pyridine was removed under reduced pressure and the resulting dark oil was triturated with saturated aqueous NaHCO3. The precipitate which formed was filtered and washed with MeOH. The material was treated with 2M HCl in Et2O to yield a gray solid, the di-HCl salt N-(6-chloro-7-fluoro-9H-β-carbolin-8-yl)-2-methyl-nicotinamide (110 mg).

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