Triethylamine → 1,3-dimethyl-6-(4-[2-(2-phenyl-4-oxo-4H-1-benzopyran-7-yl)oxyethyl]-piperazine-1-yl)-2,4(1H,3H)-pyrimidinedione

In 1.5 ml of N,N-dimethylformamide, there were reacted 0.31 g of the previously obtained 2-(2-phenyl-4-oxo-4H-1-benzopyran-7-yl)oxyethyl bromide (Compound 9), 0.2 g of 1,3-dimethyl-6-(piperazine-1-yl)-2,4(1H,3H)-pyrimidinedione (Compound 3) and 0.4 ml of triethylamine at 100° C. for 1 hour. The resultant reaction solution was poured into ice water and then extracted with chloroform. The resultant chloroform layer was then washed with water, dried over anhydrous sodium sulfate, and then concentrated under reduced pressure. Afterward, the resultant residue was recrystallized from ethanol and hexane to obtain 0.30 g (yield 68%) of 1,3-dimethyl-6-(4-[2-(2-phenyl-4-oxo-4H-1-benzopyran-7-yl)oxyethyl]-piperazine-1-yl)-2,4(1H,3H)-pyrimidinedione (the nonoxalate of Compound 10).

1. customThe resultant reaction solution
2. extractionextracted with chloroform
3. washThe resultant chloroform layer was then washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customAfterward, the resultant residue was recrystallized from ethanol and hexane

ORDレコード

ord-229b00d8eace477e849c1f2f1b21db16

出典データセット

uspto-grants-1992_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05114941