تفاعل #73424

معادلة التفاعل

4-carbomethoxytetrahydro-3-thiophenone

Formamidine acetate

sodium ethoxide

→

title compound

5,7-Dihydro-3H-thieno[3,4-d]pyrimidin-4-one

المذيبات

EtOH

ظروف التفاعل

المعالجة

1. 1
   أخرىReaction
2. 2
   درجة الحرارةis cooled to room temperature
3. 3
   تركيزconcentrated to a residue which
4. 4
   أخرىis absorbed onto silica
5. 5
   أخرىseparated via FCC (0-10% Methanol:CH2Cl2)

الإجراء التجريبي

Commercially available 4-carbomethoxytetrahydro-3-thiophenone (5 g, 31.2 mmol) is dissolved in EtOH (284 mL). Formamidine acetate (22 g, 211 mmol) is then added followed by sodium ethoxide (45 mL, 121 mmol, 21% w/w) and the mixture is heated at 90° C. for 14 hours. Reaction is cooled to room temperature and concentrated to a residue which is absorbed onto silica and separated via FCC (0-10% Methanol:CH2Cl2) to give the title compound as a solid. MS (ESI) m/z 155.14 (M+1).

المصدر