반응 #59343

반응 방정식

sodium hydroxide

cyanoacetic acid

acetic anhydride

1-isobutyl-3-methylthiourea

→

6-amino-1-isobutyl-3-methyl-2-thioxo-1H-pyrimidin-4-one

수율 29.0%

용매

ethanol

반응 조건

후처리

1. 1
   기타The solvent was evaporated
2. 2
   workup.DISSOLUTIONthe resulting red oil was redissolved in ethanol (5 mL)
3. 3
   온도The reaction mixture was refluxed for 2 h
4. 4
   기타the resulting pale brown solid was purified by flash chromatography (ethyl acetate)

실험 절차

A solution of cyanoacetic acid (1.52 g, 17.8 mmol) in acetic anhydride (2.45 mL, 25.9 mmol) was added to 1-isobutyl-3-methylthiourea (2.37 g, 16.2 mmol). The reaction mixture was heated to 60° C. for 1.5 h. The solvent was evaporated and the resulting red oil was redissolved in ethanol (5 mL) and 5M sodium hydroxide (1.6 mL, 8.1 mmol) was added. The reaction mixture was refluxed for 2 h. The solvent was co-evaporated with ethanol and the resulting pale brown solid was purified by flash chromatography (ethyl acetate) to yield 6-amino-1-isobutyl-3-methyl-2-thioxo-1H-pyrimidin-4-one (1.0 g, 29%) as a yellow solid.

출처