Sodium Iodide → 6-{4-[4-(2-Chloro-6-methlphenyl)-1-piperazinyl]-1-butenyl}-3,4-dihydrocarbostyril

温度

50 °C

2.8 Grams of 6-(4-chloro-1-butenyl)-3,4- dihydrocarbostyril and 2.1 g of sodium iodide were dissolved in 40 ml of dimethylformamide and stirred at 50° C. for 1 hour. To this solution were added 2.7 g of 4-(2-chloro-6-methlphenyl)piperazine and 1.5 g of triethylamine and the mixture was further stirred at 50° C. for 5 hours. The reaction mixture was concentrated under a reduced pressure to dryness to obtain a residue. To the residue were added 10N-NaOH and ether and stirred at a room temperature for 30 minutes to precipitate crystals. The crystals were separated by a silica-gel chromatography and recrystallized from ethanol-acetone-chloroform to obtain 6-{4-[4-(2-chloro-6-methlphenyl)-1-piperazinyl]-1-butenyl}-3,4-dihydrocarbostyril in colorless prism-like crystals. Yield: 2.7 g. Melting point: 179°-180° C.

1. stirringthe mixture was further stirred at 50° C. for 5 hours
2. concentrationThe reaction mixture was concentrated under a reduced pressure to dryness
3. customto obtain a residue
4. stirringstirred at a room temperature for 30 minutes
5. customto precipitate crystals
6. customThe crystals were separated by a silica-gel chromatography
7. customrecrystallized from ethanol-acetone-chloroform

ORDレコード

ord-9f2283ba3e644da1bb5d7d4ce69cab8b

出典データセット

uspto-grants-1984_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04455422