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Water → HCID 67492882, Verbindung

HRID 43283
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 43283
[C:1](=[O:17])(OC1C=CC([N+]([O-])=O)=CC=1)[O:2][CH2:3][CH:4]([CH3:6])[CH3:5].[NH2:18][C:19](=[NH:49])[C:20]1[CH:48]=[CH:47][C:23]([O:24][CH2:25][CH2:26][CH2:27][CH:28]2[CH2:33][CH2:32][N:31]([CH2:34][CH2:35][CH2:36][O:37][C:38]3[CH:46]=[CH:45][C:41]([C:42]([NH2:44])=[NH:43])=[CH:40][CH:39]=3)[CH2:30][CH2:29]2)=[CH:22][CH:21]=1.C(Cl)(Cl)Cl.[OH2:54]>CN(C)C=O>[NH2:49][C:19](=[N:18][C:1]([O:2][CH2:3][CH:4]([CH3:5])[CH3:6])=[O:17])[C:20]1[CH:48]=[CH:47][C:23]([O:24][CH2:25][CH2:26][CH2:27][CH:28]2[CH2:33][CH2:32][N:31]([CH2:34][CH2:35][CH2:36][O:37][C:38]3[CH:39]=[CH:40][C:41]([C:42]([NH2:44])=[N:43][C:1]([O:2][CH2:3][CH:4]([CH3:6])[CH3:5])=[O:54])=[CH:45][CH:46]=3)[CH2:30][CH2:29]2)=[CH:22][CH:21]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 962WaterHCID 6212ChloroformHCID 64292502-Methylpropyl (4-nitrophenyl) carbonateHCID 9803135T-2307 free base

Produkt 1

HCID 67492882HCID 67492882, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228
Dimethylformamide
Lösungsmittel

Versuchsvorschrift

Into a solution of 1.82 g of isobutyl 4-nitrophenyl carbonate in 15 mL of N,N-dimethylformamide, 1.50 g of 4-{3-[4-(3-{4-[amino(imino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}benzamidine was added at room temperature, and the solution was left reacting at the same temperature for 17 hours. Chloroform and water were added to the reaction mixture. The organic layer was separated, washed with water, a 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate, followed by solvent removal by evaporation under reduced pressure. The obtained residue was purified by a silica gel column chromatography (eluent; chloroform:methanol=4:1). The obtained residue was dissolved in chloroform, washed with a 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate. After removing the solvent by evaporation under reduced pressure, 1.43 g of 4-{3-[4-(3-{4-[amino(isobutoxycarbonylimino)methyl]phenoxy}propyl)-1-piperidinyl]propoxy}-N′-(isobutoxycarbonyl)benzamidine was obtained as a white solid.

Aufarbeitung

  1. waitthe solution was left
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materiala 5% potassium carbonate aqueous solution and a saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate
  5. customfollowed by solvent removal by evaporation under reduced pressure
  6. customThe obtained residue was purified by a silica gel column chromatography (eluent; chloroform:methanol=4:1)
  7. dissolutionThe obtained residue was dissolved in chloroform
  8. washwashed with a 5% potassium carbonate aqueous solution
  9. dry with materiala saturated sodium chloride aqueous solution successively, and dried over anhydrous magnesium sulfate
  10. customAfter removing the solvent
  11. customby evaporation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-7655ffef7e074a918409078dba4fa1aa
Quelldatensatz
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08536343B2

Notizen zur Reaktion

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