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Hydrochloric Acid → HCID 58193743, Verbindung

HRID 1805410
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1805410
CO[C:3]([C:5]1([C:9]#[N:10])[CH2:8][CH2:7][CH2:6]1)=[O:4].CO.[CH2:13]([NH2:16])[CH2:14][NH2:15].Cl>O>[NH2:15][CH2:14][CH2:13][NH:16][C:3]([C:5]1([C:9]#[N:10])[CH2:8][CH2:7][CH2:6]1)=[O:4]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 3301EthylenediamineHCID 25918826Methyl 1-cyanocyclobutane-1-carboxylate

Produkt 1

HCID 58193743HCID 58193743, VerbindungAusbeute 60,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962Water
Lösungsmittel

Versuchsvorschrift

8.74 g (0.063 mol) of 4 and 50 mL of methanol were mixed, after which the mixture was added dropwisely into 3.77 g (4.25 mL) of ethylene diamine to form a reaction solution. The reaction solution was subjected to reaction at room temperature for 15 hours, followed by evaporation to obtain yellow oil. The yellow oil was stirred with water and was mixed with HCl to adjust pH to 2 to obtain a crude product. The crude product was purified by placing in a column (3×20 cm) filled with 100 mL of AG 50 W×8 cationic exchange resin and elutriating with water and HCl solution having gradient concentrations, collecting an eluent fraction of a gradient concentration from 0.5 N to 1.0 N, and followed by evaporating the eluent fraction to obtain 6.37 g (0.038 mol, 60.49%) of 5.

Aufarbeitung

  1. customto form a reaction solution
  2. customThe reaction solution was subjected to reaction at room temperature for 15 hours
  3. customfollowed by evaporation
  4. customto obtain yellow oil
  5. customto obtain a crude product
  6. customThe crude product was purified
  7. additionfilled with 100 mL of AG 50 W×8 cationic exchange resin
  8. concentrationgradient concentrations
  9. customcollecting
  10. concentrationan eluent fraction of a gradient concentration from 0.5 N to 1.0 N
  11. customby evaporating the eluent fraction

Quellen und Nachweise

ORD-Eintrag
ord-8f239b632c104893b0d01703d0e69635
Quelldatensatz
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08354512B2

Notizen zur Reaktion

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