반응 #70483

반응 방정식

Triethylamine

6-chloronicotinic acid ethyl ester

(S)-2-methyl-piperazine

Water

→

desired compound

수율 52.0%

6-((S)-3-Methyl-piperazin-1-yl)-nicotinic acid ethyl ester

수율 52.0%

용매

NMP

EtOAc

반응 조건

후처리

1. 1
   기타The vial is sealed
2. 2
   기타irradiated in the microwave at 150° C. (high absorption setting) for 30 min
3. 3
   기타the organic layer is separated
4. 4
   건조dried over sodium sulfate
5. 5
   농축concentrated under reduced pressure to a white residue

실험 절차

Triethylamine (3.7 mL, 27 mmol, 5.0 eq) is added to a solution of 6-chloronicotinic acid ethyl ester (1.0 g, 5.4 mmol, 1 eq), (S)-2-methyl-piperazine (540 mg, 5.4 mmol, 1 eq) in NMP (6 mL) in a microwave vial. The vial is sealed and irradiated in the microwave at 150° C. (high absorption setting) for 30 min. Water (15 mL) and EtOAc (100 mL) are added, the organic layer is separated, dried over sodium sulfate and concentrated under reduced pressure to a white residue. The desired compound is isolated by silica gel chromatography (5-60% EtOAc/Heptane, then 10% MeOH/Heptane), (700 mg, 52% yield).

출처