Ethylamine → 2-Chloro-4-ethylamino-7-methylthieno[3,2-d]pyrimidine

温度

0 °C

In DMF was dissolved 700 mg (3.2 mmol) of 2,4-dichloro-7-methylthieno[3,2-d]pyrimidine, and then an aqueous solution of 338 mg (7.5 mmol) of ethylamine was added dropwise to the resulting solution under ice cooling over 5 minutes. The reaction mixture was stirred at 0° C. for one hour and then allowed to resume room temperature, followed by stirring for one 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=1/6) to give 524 mg (yield: 72.0%) of the title compound.

1. customto resume room temperature
2. stirringby stirring for one 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=1/6)

ORDレコード

ord-88372e7d5d2947eb8b6bcec0dfa821d1

出典データセット

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06339089B2