Sodium Carbonate → HCID 178433270, Verbindung

HRID 979928Notizen

Reaktionsgleichung

Cl.Cl[CH2:3][C:4]1[NH:8][CH:7]=[N:6][C:5]=1[CH3:9].[O:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[CH2:15][N:16]1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[N:18]=[C:17]1[NH:25][CH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.C(=O)([O-])[O-].[Na+].[Na+]>CN(C)C=O>[O:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[CH2:15][N:16]1[C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=2[N:18]=[C:17]1[NH:25][CH:26]1[CH2:27][CH2:28][N:29]([CH2:3][C:4]2[NH:8][CH:7]=[N:6][C:5]=2[CH3:9])[CH2:30][CH2:31]1

Komponenten

Reaktionsbedingungen

Temperatur: 70 °C

Versuchsvorschrift

A mixture of 3.4 parts of 5-(chloromethyl)-4-methyl-1H-imidazole monohydrochloride, 6 parts of 1-(2-furanylmethyl)-N-(4-piperidinyl)-1H-benzimidazol-2-amine, 4.25 parts of sodium carbonate and 135 parts of N,N-dimethylformamide was stirred and heated for 3 hours at 70° C. The reaction mixture was poured onto water and the product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from a mixture of acetonitrile and methanol, yielding 4.7 parts (60.2%) of 1-(2-furanylmethyl)-N-[1-[(4-methyl-1H-imidazol-5-yl)methyl]-4-piperidinyl]-1H-benzimidazol-2-amine; mp. 242.1° C. (compound 1).

Aufarbeitung

additionThe reaction mixture was poured onto water
extractionthe product was extracted with trichloromethane
customThe extract was dried
filtrationfiltered
customevaporated
customThe residue was crystallized from a mixture of acetonitrile and methanol

Quellen und Nachweise

ORD-Eintrag: ord-2a73bbde20974649b7506ceaa3b5686c
Quelldatensatz: uspto-grants-1987_01
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04634704

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