반응 #10828

반응 방정식

2,4-dimethoxy-benzoic acid hydrazide

isobutyl-isothiocyanate

→

1-(2,4-dimethoxy-benzoyl)amino-3-isobutyl-thiourea

수율 90.0%

용매

ethanol

반응 조건

후처리

1. 1
   여과The precipitate was filtered
2. 2
   세척washed with ethanol
3. 3
   기타dried in vacuo

실험 절차

Ex-109B: A solution of 2,4-dimethoxy-benzoic acid hydrazide (Ex-109A, 1.0 g, 5.1 mmol) and isobutyl-isothiocyanate (0.70 g, 6.1 mmol) in ethanol (30 mL) was refluxed for 8 hours. The precipitate was filtered, washed with ethanol, dried in vacuo to afford 1-(2,4-dimethoxy-benzoyl)amino-3-isobutyl-thiourea (1.43 g). Additional product (0.1 g, 96% overall) was obtained by concentrating the mother liquid. 1H NMR (CDCl3) δ 10.71 (bs, 1H), 9.23 (bs, 1H), 8.03 (d, J=8.6 Hz, 1H), 6.98 (bs, 1H), 6.59 (dd, J=8.6, 2.6 Hz, 1H), 6.51 (d, J=2.6 Hz, 1H), 4.02 (s, 3H), 3.86 (s, 3H), 3.41 (dd, J=6.4, 6.6 Hz, 2H), 1.96–1.87 (m, 1H), 0.91 (d, J=6.5 Hz, 6H).

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