Water → 4-(2-Pyrimidinyl)-1-piperazinebutanamine

To a cold mixture of lithium aluminum hydride (2.0 g; 5.26 mmol) and anhydrous ether (240 ml) kept at a temperature of -54° C., there was dropwise added a solution of 1-(3-cyanopropyl)-4-(2-pyrimidinyl)piperazine (8 g; 3.46 mmol) in anhydrous ether (80 ml), and the resultant mixture was kept at the same temperature as above for 1.5 hours, followed by dropwise addition of water (2 ml), a 15% aqueous potassium hydroxide solution (2 ml) and water (6 ml) in order. The reaction mixture was stirred at room temperature for 2 hours, subjected to filtration with celite and washed with chloroform. The filtrate was concentrated under reduced pressure, and the residue was purified by silica gel chromatography to give 1-(4-aminobutyl)-4-(2-pyrimidinyl)-piperazine. IR νmaxFilm (cm--1): 3100-3600, 1580, 1540.

1. customkept at a temperature of -54° C., there
2. customwas kept at the same temperature as above for 1.5 hours
3. filtrationsubjected to filtration with celite
4. washwashed with chloroform
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe residue was purified by silica gel chromatography

ORDレコード

ord-cf9a51052bbd46ffb89ef7c1054e2f6a

出典データセット

uspto-grants-1986_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04598078