تفاعل #72645

معادلة التفاعل

2-amino-4,5-dimethylthiophene-3-carbonitrile

ammonia acetate

triethyl orthobenzoate

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title compound

المردود 31.0%

5,6-Dimethyl-2-phenylthieno[2,3-d]pyrimidin-4-amine

المردود 31.0%

المذيبات

EtOAc

ظروف التفاعل

المعالجة

1. 1
   غسيلwashed with saturated NaHCO3 and H2O
2. 2
   أخرىThe solvent was removed by vacuum
3. 3
   أخرىthe residue was purified by preparative HPLC
4. 4
   غسيلeluting with acetonitrile and water

الإجراء التجريبي

A mixture of 2-amino-4,5-dimethylthiophene-3-carbonitrile (152 mg, 1.0 mmol), ammonia acetate (308.3 mg, 4.0 mmol) and triethyl orthobenzoate (2.0 mL) in a sealed tube was put in a microwave at 200° C. for 20 min. After the reaction mixture was cooled to room temperature, it was diluted with EtOAc, washed with saturated NaHCO3 and H2O. The solvent was removed by vacuum and the residue was purified by preparative HPLC eluting with acetonitrile and water to give the title compound (80 mg, 31%). 1H NMR (400 MHz, CDCl3) δ2.45 (s, 3H), 2.48 (s, 3H), 5.34 (bs, 2H), 7.46-7.43 (m, 3H), 8.4-8.38 (m, 2H). MS 256 (MH+).

المصدر