Triethylamine → 4-(3-Hydroxypropyl)-1-[4-[1-[3-(isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoyl]piperazine

1-[4-[1-[3-(Isopropylamino)-2-pyridyl]piperazin-4-yl-carbonyl]benzoyl]piperazine (0.5 g) was dissolved in anhydrous ethanol (25 ml) and then, triethylamine (0.3 ml) and 3-bromo-1-propanol (0.5 g) were added. The solution was heated to reflux for 12 hours. The solvent was concentrated under reduced pressure and then, the residue was dissolved in chloroform (50 ml), and the solution was washed with water twice. Water (40 ml), methanol (5 ml) and aqueous 10% sodium hydroxide (10 ml) were added to chloroform solution and the mixture was stirred for 1 hour. The separated organic layers were washed with water and the solvent was concentrated under reduced pressure. The concentrated residue was crystallized by treatment with ether, and further recrystallized using ethyl acetate and ether, filtered and dried to give 0.44 g (yield: 78%) of the desired compound as white crystal.

1. temperatureThe solution was heated
2. temperatureto reflux for 12 hours
3. concentrationThe solvent was concentrated under reduced pressure
4. dissolutionthe residue was dissolved in chloroform (50 ml)
5. washthe solution was washed with water twice
6. additionWater (40 ml), methanol (5 ml) and aqueous 10% sodium hydroxide (10 ml) were added to chloroform solution
7. washThe separated organic layers were washed with water
8. concentrationthe solvent was concentrated under reduced pressure
9. customThe concentrated residue was crystallized by treatment with ether
10. customfurther recrystallized
11. filtrationfiltered
12. customdried

ORDレコード

ord-44dfe2c8848440c1b6caafd07e37336b

出典データセット

uspto-grants-1999_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05922871