Hydrochloric Acid → 7-Chloro-4-[[4-[[[1-(phenylmethyl)-4-piperidinyl]amino]carbonyl]phenyl]amino]-3-quinolinecarboxylic acid

7-Chloro-4-[[4-[[[1-(phenylmethyl)-4piperidinyl]amino]carbonyl]phenyl]amino]-3-quinolinecarboxylic acid ethyl ester (51.7 g, 95.2 mmol) was stirred in 550 ml of methanol and treated with 133 ml of 2.5 M NaOH. The reaction mixture was then refluxed for 45 m at which point the hot homogeneous solution was treated with 166 ml of 2 M HCl to precipitate the product. After the mixture cooled to room temperature, the product was filtered and washed with water, methanol and then ether. The yellow powdery material was then dried in vacuo overnight affording 31.3 g (60.9 mmol, 64% yield) of 7-chloro-4-[[4-[[[1-(phenylmethyl)-4-piperidinyl]amino]carbonyl]phenyl]amino]-3-quinolinecarboxylic acid.

1. temperatureThe reaction mixture was then refluxed for 45 m at which point the hot homogeneous solution
2. customto precipitate the product
3. filtrationthe product was filtered
4. washwashed with water, methanol
5. customThe yellow powdery material was then dried in vacuo overnight

ORDレコード

ord-047bc975c67d4e79a9331ccde7b92feb

出典データセット

uspto-grants-1995_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05438064