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Sodium Hydroxide → HCID 13049055, Verbindung

HRID 1390627
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1390627
[N+]([NH:4][C:5]([NH2:7])=[O:6])([O-])=O.[N:8]1([CH2:14][CH2:15][O:16][CH:17]2[CH2:21][CH2:20]N[CH2:18]2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.[OH-].[Na+]>C(O)C>[N:8]1([CH2:14][CH2:15][O:16][CH:17]2[CH2:21][CH2:20][N:4]([C:5]([NH2:7])=[O:6])[CH2:18]2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 62372NitroureaHCID 2133316470001-70-6

Produkt 1

HCID 13049055HCID 13049055, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

Nitrourea (7.3 g., 0.055 mole of 80% wet reagent) and 3-(2-piperidinoethoxy)pyrrolidine were stirred together in 100 ml. ethanol at reflux for 2 hr. After cooling, the reaction mixture was filtered and the filtrate concentrated to give 12.5 g. solid material which was determined by nuclear magnetic resonance spectrum analysis to be a salt. The crude product was treated with dilute sodium hydroxide solution and the free base extracted into chloroform twice. The chloroform extracts were combined, washed with water, dried over magnesium sulfate, filtered, and concentrated to give 6.8 g. of off-white solid product. Recrystallization from isopropyl ether-isopropanol gave 3.7 g. (30.7%) white solid, m.p. 133.5°-135.5° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe reaction mixture was filtered
  3. concentrationthe filtrate concentrated
  4. customto give 12.5 g
  5. extractionthe free base extracted into chloroform twice
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customto give 6.8 g
  11. customRecrystallization from isopropyl ether-isopropanol
  12. customgave 3.7 g

Quellen und Nachweise

ORD-Eintrag
ord-e258341b699d45c2a4a1ec8e6c51ab1f
Quelldatensatz
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04139620

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