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1-Bromo-3-chloropropane → HCID 12899443, Verbindung

HRID 621553
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 621553
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Br:13])[C:11]=1[OH:12])[NH:8][C:7](=[O:14])[CH2:6][CH2:5]2.[OH-].[Na+].Br[CH2:18][CH2:19][CH2:20][Cl:21]>C(O)(C)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[C:10]([Br:13])[C:11]=1[O:12][CH2:18][CH2:19][CH2:20][Cl:21])[NH:8][C:7](=[O:14])[CH2:6][CH2:5]2
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 80061-Bromo-3-chloropropaneHCID 14798Sodium HydroxideHCID 21243036HCID 21243036, Verbindung

Produkt 1

HCID 12899443HCID 12899443, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

5 grams of 6-chloro-8-bromo-7-hydroxy-3,4-dihydrocarbostyril and 3 g of sodium hydroxide are mixed with 120 ml of isopropanol and stirred at 50°-60° C. for 1 hour. Then 10 ml of 3-bromo-1-chloropropane are added thereto and stirred at 70°-80° C. for 6 hours. The reaction mixture is concentrated under reduced pressure to dryness and the residue thus obtained is extracted with chloroform. The chloroform layer is washed with water and dried. Then chloroform is removed by distillation and the residue thus formed is recrystallized from ethanol to obtain 6.2 g of 6-chloro-8-bromo-7-(3-chloropropoxy)-3,4-dihydrocarbostyril in the form of colorless needle-like crystals with a melting point of 87°-88° C.

Aufarbeitung

  1. stirringstirred at 70°-80° C. for 6 hours
  2. concentrationThe reaction mixture is concentrated under reduced pressure to dryness
  3. customthe residue thus obtained
  4. extractionis extracted with chloroform
  5. washThe chloroform layer is washed with water
  6. customdried
  7. customThen chloroform is removed by distillation
  8. customthe residue thus formed
  9. customis recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-e09a748330134ccc891cc652b2bc3323
Quelldatensatz
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04824840

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