Triethylamine → 2-Chloro-4-(2-carbamoylethylamino)-7-methylthieno[3,2-d]pyrimidine

温度

0 °C

In 10 ml of DMF, 1.0 g (4.9 mmol) of 2,4-dichloro-7-methylthieno[3,2-d]pyrimidine was dissolved, and then 668 mg (5.37 mmol) of β-alanineamide hydrochloride and 1.09 g (10.7 mmol) of triethylamine were added thereto under ice cooling. The reaction solution was stirred at 0° C. for one hour and then allowed to resume room temperature, followed by stirring for further 1 hour. After completion of the reaction, ice water was added to the reaction mixture, followed by extraction with ethyl acetate (50 ml×3). After the organic layer was washed successively with 1N hydrochloric acid, water and brine and dried over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/8) to give 1.05 g (yield: 79.8%) of the title compound.

1. customto resume room temperature
2. stirringby stirring for further 1 hour
3. additionwas added to the reaction mixture
4. extractionfollowed by extraction with ethyl acetate (50 ml×3)
5. washAfter the organic layer was washed successively with 1N hydrochloric acid, water and brine
6. dry with materialdried over anhydrous sodium sulfate
7. distillationthe solvent was distilled off under reduced pressure
8. customThe residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/8)

ORDレコード

ord-064543062e254504b9e2a0586f065070

出典データセット

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06339089B2