반응 #464555

반응 방정식

benzothiophen-2-carboxylic acid

N-methylpiperazine dihydrochloride

N-methylpiperazine

→

pure title compound

수율 70.9%

Benzothiophen-2-carboxaldehyde

수율 70.9%

용매

THF

THF

반응 조건

후처리

1. 1
   온도The mixture was refluxed for 4 hours

실험 절차

LiA1H4 (7.6 g, 200 mmol) was suspended under stirring at 0° under Ar in anhydrous THF (400 ml), then N-methylpiperazine dihydrochloride (17.3 g, 100 mmol) was added portionwise in 10 min. N-methylpiperazine (30 g, 300 mmol) was then added dropwise, the mixture was warmed to RT and stirring continued for 2 hours. The surnatant of this suspension was then added by syringe to a stirred solution at 0° under Ar of benzothiophen-2-carboxylic acid (7.13 g, 40.0 mmol) in anhydrous THF (200 ml). The mixture was refluxed for 4 hours and after the same procedure as in preparation 6 pure title compound was obtained (4.6 g, 28.4 mmol, yield 70.9%) as dark orange crystals.

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