반응 #71681

반응 방정식

3-methyl-4-{[(3S)-3-methyl-1-piperazinyl]sulfonyl}benzonitrile

6-methyl-3-pyridinecarboxylic acid

DIPEA

HATU

→

NH3

title compound

3-Methyl-4-({(3S)-3-methyl-4-[(6-methyl-3-pyridinyl)carbonyl]-1-piperazinyl}sulfonyl)benzonitrile

용매

MeOH

DCM

DMF

반응 조건

후처리

1. 1
   농축Concentration in vacuo
2. 2
   기타gave a yellow oil, that
3. 3
   기타was purified by MDAP purification
4. 4
   기타concentration of the desired fractions gave a clear film (78.8 mg)

실험 절차

To a solution of 3-methyl-4-{[(3S)-3-methyl-1-piperazinyl]sulfonyl}benzonitrile (Description 11) (75 mg, 0.268 mmol), 6-methyl-3-pyridinecarboxylic acid (40.5 mg, 0.295 mmol) and DIPEA (0.070 ml, 0.403 mmol) in dry DMF (3 ml) at room temperature under Ar was added HATU (122 mg, 0.322 mmol) and the resulting yellow solution stirred at room temperature for 1 h. Concentration in vacuo gave a yellow oil, that was purified by MDAP purification; concentration of the desired fractions gave a clear film (78.8 mg). Flash chromatography (silica; Flash 12S; linear gradient (1-8%) [2M NH3 in MeOH] in DCM) gave the title compound as a clear film (54.5 mg) that became a white solid on standing in vacuo (1 mbar) for 1 hour.

출처