تفاعل #59343

معادلة التفاعل

sodium hydroxide

cyanoacetic acid

acetic anhydride

1-isobutyl-3-methylthiourea

→

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

المردود 29.0%

المذيبات

ethanol

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر