Hydrochloric Acid → 4'-[4-[4-(cis-2,6-Dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1'-biphenyl-4-carboxylic acid

HRID 1816756Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1816756
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][C:14]([N:17]3[CH2:22][CH2:21][N:20]([C:23]4[CH:28]=[CH:27][C:26]([N:29]5[CH2:34][C@H:33]([CH3:35])[O:32][C@H:31]([CH3:36])[CH2:30]5)=[CH:25][CH:24]=4)[CH2:19][CH2:18]3)=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)=[O:4].[OH-].[Na+].CO.Cl>O.O1CCCC1>[CH3:35][C@H:33]1[O:32][C@@H:31]([CH3:36])[CH2:30][N:29]([C:26]2[CH:25]=[CH:24][C:23]([N:20]3[CH2:19][CH2:18][N:17]([C:14]4[CH:15]=[CH:16][C:11]([C:8]5[CH:9]=[CH:10][C:5]([C:3]([OH:4])=[O:2])=[CH:6][CH:7]=5)=[CH:12][CH:13]=4)[CH2:22][CH2:21]3)=[CH:28][CH:27]=2)[CH2:34]1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 14798Sodium HydroxideHCID 538200644'-[4-[4-(cis-2,6-Dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1'-biphenyl-4-carboxylic acid methyl ester

Produkt 1

HCID 538355204'-[4-[4-(cis-2,6-Dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1'-biphenyl-4-carboxylic acidAusbeute 102,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 4′-[4-[4-(cis-2,6-dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1′-biphenyl-4-carboxylic acid methyl ester (3.70 g) and 1.0 mol/l sodium hydroxide solution (30 ml) in a mixed solvent of methanol (75 ml) and tetrahydrofuran (185 ml) was refluxed for 15.5 hours. After cooling to ambient temperature, the reaction mixture was poured into cold water, and the mixture was adjusted to pH 2 with 1.0 mol/l hydrochloric acid. The resulting precipitates were filtered, washed with water and diisopropyl ether and dried to give 4′-[4-[4-(cis-2,6-dimethylmorpholin-4-yl)phenyl]piperazin-1-yl]-1,1′-biphenyl-4-carboxylic acid (3.68 g).

Aufarbeitung

  1. temperaturewas refluxed for 15.5 hours
  2. customThe resulting precipitates
  3. filtrationwere filtered
  4. washwashed with water and diisopropyl ether
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2ca87cb8a54e4f1c9b51de002c1fd3ba
Quelldatensatz
uspto-grants-2005_04
Patentnummer
US06884868B1

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