Hydrochloric Acid → 5-[2-Hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydro carbostyril monohydrochloride

HRID 569955ノート

反応式

HRID 569955 の反応式
[O:1]1[CH2:16][CH:2]1[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[CH2:7][CH2:8][C:9](=[O:15])[NH:10]2.[C:17]1([N:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[ClH:29].C(O)C>CO.CC(C)=O>[ClH:29].[OH:1][CH:2]([CH2:16][N:26]1[CH2:27][CH2:28][N:23]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:24][CH2:25]1)[CH2:3][O:4][C:5]1[CH:14]=[CH:13][CH:12]=[C:11]2[C:6]=1[CH2:7][CH2:8][C:9](=[O:15])[NH:10]2

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 70961-PhenylpiperazineHCID 128994235-[(Oxiran-2-yl)methoxy]-3,4-dihydroquinolin-2(1H)-one

生成物 1

HCID 128994275-[2-Hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydro carbostyril monohydrochloride

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 887Methanol溶媒

実験手順

4.4 Grams of 5-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril and 3.4 g of 4-phenylpiperazine are dispersed in 60 ml of methanol and reacted at 50°-60° C. for 3 hours. After the reaction is completed, the reaction mixture is concentrated under a reduced pressure. To the residue thus obtained are added 5 ml of concentrated hydrochloric acid and 30 ml of ethanol to dissolve the residue uniformly and further 200 ml of acetone are added. The crystals precipitated are collected by filtration and dried. Recrystallization from water obtains 6.5 g of 5-[2-hydroxy-3-(4-phenylpiperazinyl)propoxy]-3,4-dihydrocarbostyril monohydrochloride in the form of colorless needle-like crystals with a melting point of 239°-241° C.

後処理

  1. customreacted at 50°-60° C. for 3 hours
  2. concentrationthe reaction mixture is concentrated under a reduced pressure
  3. customTo the residue thus obtained
  4. dissolutionto dissolve the residue uniformly
  5. customThe crystals precipitated
  6. filtrationare collected by filtration
  7. customdried
  8. customRecrystallization from water

出典と根拠

ORDレコード
ord-f448c440e4f4405484860cae6cb7d71e
出典データセット
uspto-grants-1988_03
特許番号
US04734416

反応ノート

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