Sodium Hydroxide → 3-{3-[4-(diphenylmethyl)-1-piperazinyl]-propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetic acid hemihydrate

HRID 2050327

Reaktionsgleichung

Reaktionsgleichung von HRID 2050327
[C:1]1([CH:7]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N:19]([CH2:26][C:27]([O:29]CC)=[O:28])[C:18]3=[O:32])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>O>[OH2:28].[C:33]1([CH:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N:19]([CH2:26][C:27]([OH:29])=[O:28])[C:18]3=[O:32])[CH2:12][CH2:13]2)[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1.[C:1]1([CH:7]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17]3[C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][C:20]=4[N:19]([CH2:26][C:27]([OH:29])=[O:28])[C:18]3=[O:32])[CH2:10][CH2:9]2)[C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 20506279ethyl 3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetate

Produkt 1

HCID 887389743-{3-[4-(diphenylmethyl)-1-piperazinyl]-propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetic acid hemihydrate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 9.8 parts of ethyl 3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetate, 1.2 parts of sodium hydroxide and 150 parts of water is stirred and refluxed for 5 minutes (+80° C.). The reaction mixture is filtered and the filtrate is acidified with acetic acid to pH 5.8-6; a sticky precipitate is formed. It is separated and crystallized from ethanol and water. The product is filtered off and dried in vacuo at 100° C. for 3 hours, yielding 6 parts of 3-{3-[4-(diphenylmethyl)-1-piperazinyl]propyl}-2,3-dihydro-2-oxo-1H-benzimidazole-1-acetic acid hemihydrate; mp. 138.7° C.

Aufarbeitung

  1. temperaturerefluxed for 5 minutes (+80° C.)
  2. filtrationThe reaction mixture is filtered
  3. customa sticky precipitate is formed
  4. customIt is separated
  5. customcrystallized from ethanol and water
  6. filtrationThe product is filtered off
  7. customdried in vacuo at 100° C. for 3 hours

Quellen und Nachweise

ORD-Eintrag
ord-aac17a2480a64d67aeedc4c0558635c5
Quelldatensatz
uspto-grants-1980_04
Patentnummer
US04200641

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