Sodium Cyanide → HCID 12852741, Verbindung

HRID 1105884Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1105884
Cl[C:2]1[S:6][N:5]([CH2:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:4](=[O:15])[CH:3]=1.[C-:16]#[N:17].[Na+]>C(Cl)(Cl)Cl.O.[Br-].C([N+](CCCC)(CCCC)CCCC)CCC>[C:16]([C:2]1[S:6][N:5]([CH2:7][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:4](=[O:15])[CH:3]=1)#[N:17]

Komponenten

6

Edukt 2

HCID 8929Sodium CyanideHCID 13013787HCID 13013787, Verbindung

Produkt 1

HCID 12852741HCID 12852741, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 74236Tetrabutylammonium BromideKatalysatorHCID 962WaterLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A mixture of 4.8 g. (0.02 mole) of 5-chloro-2-phenethyl-4-isothiazolin-3-one in 25 ml of CHCl3, 1.0 g. (0.02 mole) of sodium cyanide in 5 ml of water and 0.015 g of tetrabutyl ammonium bromide was heated under reflux for 1 hour, while stirring. The mixture was then washed with water, dried, and concentrated to give a gummy brown residue, which was recrystallized from 300 ml of ethanol to give 0.15 g. of the named product, mp 228°-230 (softened at 210°).

Aufarbeitung

  1. additionA mixture of 4.8 g
  2. temperatureunder reflux for 1 hour
  3. washThe mixture was then washed with water
  4. customdried
  5. concentrationconcentrated
  6. customto give a gummy brown residue, which
  7. customwas recrystallized from 300 ml of ethanol
  8. customto give 0.15 g
  9. custom230 (softened at 210°)

Quellen und Nachweise

ORD-Eintrag
ord-15c025393f174b258986b72caac078b0
Quelldatensatz
uspto-grants-1982_01
Patentnummer
US04310590

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