반응 #3214

반응 방정식

2-aminobenzonitrile

dimethyl acetylenedicarboxylate

→

solid

수율 44.3%

Dimethyl 2-(2-cyanoanilino)fumarate

수율 44.3%

용매

t-butanol

반응 조건

후처리

1. 1
   기타a precipitate formed
2. 2
   여과was collected by filtration
3. 3
   세척The material was washed with cold methanol and air
4. 4
   기타dried

실험 절차

A solution of 2-aminobenzonitrile (5.00 g, 42.3 mM) and dimethyl acetylenedicarboxylate (6.42 g, 45.2 mM) in t-butanol (70.5 mL) was refluxed under a nitrogen atmosphere for 12 hr. After cooling the reaction mixture to room temperature, a precipitate formed and was collected by filtration. The material was washed with cold methanol and air dried to give a yellow solid (4.88 g). Recrystallization of this solid from methanol provided the title compound (4.39 g, 39.9%) as yellow crystals, mp 116.5°-117.5° C.; MS(CI): 261 (M+H). Analysis for C13H12N2O4 : Calculated: C, 60.00; H, 4.65; N, 10.76 Found: C, 60.03; H, 4.67; N, 10.84

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