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Water → 4-(4-Nitro-3-trifluoromethyl-phenylamino)-piperidine-1-carboxylic acid [1-(4-ethoxy-phenyl)-piperidin-4-ylmethyl]-methyl-amide

HRID 511151
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 511151
ClC(Cl)(O[C:5](=[O:11])OC(Cl)(Cl)Cl)Cl.[CH3:13][NH:14][CH2:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][C:25](C(F)(F)F)=[CH:24][CH:23]=2)[CH2:18][CH2:17]1.C(N([CH2:37][CH3:38])CC)C.[N+:39]([C:42]1[CH:47]=[CH:46][C:45]([NH:48][CH:49]2[CH2:54][CH2:53][NH:52][CH2:51][CH2:50]2)=[CH:44][C:43]=1[C:55]([F:58])([F:57])[F:56])([O-:41])=[O:40].[OH2:59]>C(#N)C>[CH2:37]([O:59][C:25]1[CH:24]=[CH:23][C:22]([N:19]2[CH2:18][CH2:17][CH:16]([CH2:15][N:14]([CH3:13])[C:5]([N:52]3[CH2:51][CH2:50][CH:49]([NH:48][C:45]4[CH:46]=[CH:47][C:42]([N+:39]([O-:41])=[O:40])=[C:43]([C:55]([F:58])([F:56])[F:57])[CH:44]=4)[CH2:54][CH2:53]3)=[O:11])[CH2:21][CH2:20]2)=[CH:27][CH:26]=1)[CH3:38]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 962WaterHCID 8471TriethylamineHCID 94429TriphosgeneHCID 43448257N-(4-Nitro-3-(trifluoromethyl)phenyl)piperidin-4-amineHCID 62648464Methyl-[1-(4-trifluoromethyl-phenyl)-piperidin-4-ylmethyl]-amine

Produkt 1

HCID 58576857
4-(4-Nitro-3-trifluoromethyl-phenylamino)-piperidine-1-carboxylic acid [1-(4-ethoxy-phenyl)-piperidin-4-ylmethyl]-methyl-amide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel2×

Versuchsvorschrift

Triphosgene (60 mg; 0.20 mmol) is added to a solution of methyl-[1-(4-trifluoromethyl-phenyl)-piperidin-4-ylmethyl]-amine (150 mg; 0.60 mmol) and triethylamine (185 μL; 1.33 mmol) in acetonitrile (6 mL). After stirring for 15 minutes a solution of (4-nitro-3-trifluoromethyl-phenyl)-piperidin-4-yl-amine (173 mg; 0.60 mmol, in acetonitrile (10 mL) is added. After 2 hours reaction time at room temperature, the mixture is poured into water (10 m) and the aqueous layer is extracted with ethyl acetate (3×50 mL). The combined organic layers are dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude product is purified by column chromatography on silica gel (Ethyl acetate:heptane 8:2) to afford the desired product (267 mg; 0.45 mmol). The structure was confirmed using Protocol II-E. Calculated mass=564; observed mass=564; HPLC retention time=7.73 min.

Aufarbeitung

  1. customAfter 2 hours reaction time at room temperature
  2. extractionthe aqueous layer is extracted with ethyl acetate (3×50 mL)
  3. dry with materialThe combined organic layers are dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude product is purified by column chromatography on silica gel (Ethyl acetate:heptane 8:2)

Quellen und Nachweise

ORD-Eintrag
ord-6e820a468081423999eb4ce5a2f5ffd6
Quelldatensatz
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09096524B2

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