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Dimethylformamide → HCID 21193267, Verbindung

HRID 1068459
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1068459
C(OC([N:8]1[CH2:16][CH2:15][C:11]([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[CH:19]=2)([C:12](O)=[O:13])[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.CN(C)[CH2:28][CH2:29][CH2:30]N=C=NCC.[OH2:37].ON1C2C=CC=CC=2N=N1.[Cl-].[NH4+:49].[CH:50](N(C(C)C)CC)(C)C.CN(C)[CH:61]=[O:62]>>[C:29]([O:37][C:61]([NH:49][C:12](=[O:13])[C:11]1([CH2:17][C:18]2[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[CH:19]=2)[CH2:15][CH2:16][NH:8][CH2:9][CH2:10]1)=[O:62])([CH3:30])([CH3:50])[CH3:28]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 6

HCID 6228DimethylformamideHCID 25517Ammonium ChlorideHCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 211933671-Boc-4-(3-methylbenzyl)-4-carboxypiperidine

Produkt

1
HCID 21193267HCID 21193267, Verbindung

Versuchsvorschrift

A mixture of N-tert-butoxycarbonyl-4-(3-methylbenzyl)-isonipecotic acid (1.02 g, 3.00 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.64 g. 3.36 mmol), 1-hydroxy-benzotriazole hydrate (0.45 g, 3.31 mmol), ammonium chloride (0.33 g, 6.15 mmol), and diisopropylethylamine (1.15 mL, 6.60 mmol) in anhydrous dimethylformamide (10 ml) was stirred at room temp. overnight. The resultant solution was concentrated under vacuum and the residue was partitioned between ethyl acetate and water. The organic extracts were combined, washed with brine, dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residual oil was subjected to column chromatography on silica eluting with 40% ethyl acetate in hexane. Collection and concentration of appropriate fractions provided the title product.

Aufarbeitung

  1. concentrationThe resultant solution was concentrated under vacuum
  2. customthe residue was partitioned between ethyl acetate and water
  3. washwashed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customCollection and concentration of appropriate fractions

Quellen und Nachweise

ORD-Eintrag
ord-a352930e26614ea9ba4ac728620a1cec
Quelldatensatz
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06248756B1

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