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1,2-Dichloroethane → HCID 11754542, Verbindung

HRID 225773
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 225773
C(Cl)CCl.C(N(C(C)C)CC)(C)C.C(N)C1C=CC=CC=1.[CH3:22][C:23]1[CH:39]=[CH:38][C:26]([C:27]([N:29]2[CH2:34][CH2:33][CH2:32][CH2:31][CH:30]2[C:35](O)=O)=[O:28])=[CH:25][CH:24]=1.[CH2:40]([NH:47][C:48]([C:50]1[CH:55]=[CH:54][C:53]([Cl:56])=[CH:52][C:51]=1[NH-:57])=[O:49])[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1>>[CH2:40]([N:47]1[C:48](=[O:49])[C:50]2[C:51](=[CH:52][C:53]([Cl:56])=[CH:54][CH:55]=2)[N:57]=[C:35]1[CH:30]1[CH2:31][CH2:32][CH2:33][CH2:34][N:29]1[C:27](=[O:28])[C:26]1[CH:38]=[CH:39][C:23]([CH3:22])=[CH:24][CH:25]=1)[C:41]1[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 5

HCID 111,2-DichloroethaneHCID 7504BenzylamineHCID 81531DiisopropylethylamineHCID 167698421-(4-Methylbenzoyl)piperidine-2-carboxylic acidHCID 178514215HCID 178514215, Verbindung

Produkt 1

HCID 11754542HCID 11754542, Verbindung
Ausbeute 47 %

Versuchsvorschrift

Formula 205 where T is a covalent bond; W, X, Y and Z are —C═; U—V is —N(R6)—CReRf—CRgRh—; R1, R2, R4 and Ra to Rh are H; Rand R6 is p-methyl-benzoyl: A mixture of the compound of Formula 203 (2.66 g, 6.7 mmol), 1M NaOH (27 mL), methanol (54 mL), and dioxane (36 mL) was stirred at room temperature for 7 hours. The solvents were evaporated and the residue portioned between dichloromethane (75 mL), saturated NaCl (50 mL), and concentrated HCl (3 mL). The layers were separated and the organic layer dried over MgSO4 and concentrated under vacuum to give the corresponding compound of Formula 204, 4-chloro-2-[1-(4-methyl-benzoyl)-piperidine-2-carbonyl]amino}-benzoic acid, which was carried forward without further purification. This crude product was redissolved in dichloromethane and treated with EDC (3.84 g, 20 mmol), and diisopropylethylamine (3.50 mL, 20 mmol). After stirring 20 minutes, benzylamine (2.20 mL, 20 mmol) was added and the mixture stirred overnight at room temperature. The mixture was washed with water (2×50 mL) and 1M HCl, dried over MgSO4, filtered and concentrated under vacuum to give 1.5 g (47% yield) of the desired product of Formula 205, 1-(4-methyl-benzoyl)-piperidine-2-carboxylic acid (2-benzylcarbamoyl-5-chloro-phenyl-amide, a crude product that was found to be 80% pure by reverse phase HPLC. The product was taken on without further purification. LRMS (MH+) m/z 491.

Aufarbeitung

  1. customwas carried forward without further purification
  2. dissolutionThis crude product was redissolved in dichloromethane
  3. stirringthe mixture stirred overnight at room temperature
  4. washThe mixture was washed with water (2×50 mL) and 1M HCl
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-879cb533180c4014998c1edc2da0fde4
Quelldatensatz
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07557115B2

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