반응 #40501

반응 방정식

EtOAc

6-chloro-4-methyl-9H-β-carbolin-8-ylamine

Nicotinoyl chloride hydrochloride

→

N-(6-chloro-4-methyl-9H-β-carbolin-8-yl)-nicotinamide

수율 8.1%

용매

H2O

pyridine

H2O

반응 조건

후처리

1. 1
   workup.ADDITIONpoured into a separatory funnel
2. 2
   workup.STIRRINGThe reaction mixture was shaken
3. 3
   기타the layers were separated
4. 4
   추출The aqueous layer was extracted with EtOAc (2×25 ml)
5. 5
   세척The combined organic layers were washed with a saturated sodium bicarbonate solution (15 ml)
6. 6
   건조dried over MgSO4
7. 7
   여과filtered
8. 8
   농축concentrated

실험 절차

A solution of 6-chloro-4-methyl-9H-β-carbolin-8-ylamine (43 mg, 0.19 mmol) in pyridine (4 ml) was stirred at RT under an argon atmosphere. Nicotinoyl chloride hydrochloride (40 mg, 0.22 mmol) was added thereto and the reaction mixture was stirred for 12 hr. The solution was diluted with H2O (5 ml) and poured into a separatory funnel containing H2O (5 ml) and EtOAc (25 ml). The reaction mixture was shaken and the layers were separated. The aqueous layer was extracted with EtOAc (2×25 ml). The combined organic layers were washed with a saturated sodium bicarbonate solution (15 ml), followed by brine, then dried over MgSO4, filtered, and concentrated to yield N-(6-chloro-4-methyl-9H-β-carbolin-8-yl)-nicotinamide (5.2 mg) as an orange viscous oil.

출처