Dicyclohexylcarbodiimide → Manidipine

HRID 1475169

Reaktionsgleichung

[CH3:1][O:2][C:3]([C:5]1[CH:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=2)[C:9]([C:20]([OH:22])=[O:21])=[C:8]([CH3:23])[NH:7][C:6]=1[CH3:24])=[O:4].C1(N=C=NC2CCCCC2)CCCCC1.CN(C1C=CC=CN=1)C.[CH:49]([N:62]1[CH2:67][CH2:66][N:65]([CH2:68][CH2:69]O)[CH2:64][CH2:63]1)([C:56]1[CH:61]=[CH:60][CH:59]=[CH:58][CH:57]=1)[C:50]1[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=1>C1(C)C=CC=CC=1>[CH3:24][C:6]1[NH:7][C:8]([CH3:23])=[C:9]([C:20]([O:22][CH2:69][CH2:68][N:65]2[CH2:64][CH2:63][N:62]([CH:49]([C:56]3[CH:57]=[CH:58][CH:59]=[CH:60][CH:61]=3)[C:50]3[CH:51]=[CH:52][CH:53]=[CH:54][CH:55]=3)[CH2:67][CH2:66]2)=[O:21])[CH:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-:19])=[O:18])[CH:12]=2)[C:5]=1[C:3]([O:2][CH3:1])=[O:4]

Komponenten

Reaktionsbedingungen

Temperatur: 72.5 °C

Versuchsvorschrift

To a suspension of 2,6-dimethyl-4-(3-nitro-phenyl)-1,4-dihydro-pyridine-3,5-dicarboxylic acid monomethyl ester (5 gm), dicyclohexyl carbodiimide (3.08 gm) and dimethylamino pyridine (0.25 gm) in toluene (30 ml) at room temperature was added 2-(4-benzhydryl piperazine-1-yl)ethanol (7.5 gm). Reaction mass was then heated to 70-75° C. for 2 hours. Reaction mass was then cooled to room temperature and filtered. Toluene layer was concentrated under vacuum to get manidipine base (5 gm).

Aufarbeitung

customReaction mass
customReaction mass
temperaturewas then cooled to room temperature
filtrationfiltered
concentrationToluene layer was concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag: ord-560eb7a71ae64a37af1fd5388192132e
Quelldatensatz: uspto-grants-2015_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US09018376B2

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