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Epichlorohydrin → HCID 12899440, Verbindung

HRID 1979763
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1979763
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([OH:13])=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2.C(=O)([O-])[O-].[K+].[K+].[CH2:20]([CH:22]1[O:24][CH2:23]1)Cl.[OH-].[Na+]>C(O)(C)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:13][CH2:20][CH:22]2[O:24][CH2:23]2)=[C:6]2[C:11]=1[NH:10][C:9](=[O:12])[CH2:8][CH2:7]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 7835EpichlorohydrinHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 12899415HCID 12899415, Verbindung

Produkt 1

HCID 12899440HCID 12899440, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776Isopropanol
Lösungsmittel

Versuchsvorschrift

20.0 Grams of 8-bromo-5-hydroxy-3,4-dihydrocarbostyril and 18 g of potassium carbonate were dispersed in 160 ml of isopropanol, then 40 ml of epichlorohydrin was added thereinto and reacted at 80° C. for 6 hours. The reaction mixture was concentrated under a reduced pressure and to the residue thus obtained was added 100 ml of 2N-sodium hydroxide and stirred well. The insoluble matters formed were obtained by filtration and washed with water and dried to obtain crude crystals. Recrystallization of the crude crystal from methanol to obtain 18.5 g of 8-bromo-5-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril as in the form of colorless needle-like crystals. Melting point: 220°-220° C.

Aufarbeitung

  1. customreacted at 80° C. for 6 hours
  2. concentrationThe reaction mixture was concentrated under a reduced pressure and to the residue
  3. customthus obtained
  4. customThe insoluble matters formed
  5. customwere obtained by filtration
  6. washwashed with water
  7. customdried
  8. customto obtain crude crystals
  9. customRecrystallization of the crude crystal from methanol

Quellen und Nachweise

ORD-Eintrag
ord-7f68d63a85dd4776989d5324d086d316
Quelldatensatz
uspto-grants-1984_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04482560

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