Water → HCID 54343145, Verbindung

HRID 342749Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 342749
Cl[CH2:2][C:3](=[O:18])[C:4]([NH:7][C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[CH:10]=1)([CH3:6])[CH3:5].[C-:19]#[N:20].[Na+].O.C(Cl)Cl>C(#N)C.C1OCCOCCOCCOCCOCCOC1>[C:19]([CH2:2][C:3](=[O:18])[C:4]([NH:7][C:8](=[O:17])[C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[CH:10]=1)([CH3:6])[CH3:5])#[N:20]

Komponenten

7

Edukt 4

HCID 962WaterHCID 6344DichloromethaneHCID 8929Sodium CyanideHCID 54029353HCID 54029353, Verbindung

Produkt 1

HCID 54343145HCID 54343145, VerbindungAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 2855718-Crown-6KatalysatorHCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

N-(3'-chloro-1',1'-dimethylacetonyl)-3,5-dichlorobenzamide (30 gm, 0.0972 m), sodium cyanide (15 gm, 0.306 m) and 18-crown-6 (1 gm) were dissolved in 300 ml of acetonitrile in a round bottom flask under a nitrogen atmosphere. The mixture was heated to reflux for about 4 hours. The contents of the flask were then cooled and transferred to a separatory funnel along with 100 ml of water and 500 ml of methylene chloride and mixed well. The aqueous layer was discarded and the organic layer was washed sequentially with water and brine, dried and the solvents stripped off to yield 12.5 gm of the product after recrystallization from methylene chloride and hexane.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux for about 4 hours
  3. temperatureThe contents of the flask were then cooled
  4. additionmixed well
  5. washthe organic layer was washed sequentially with water and brine
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-8917dc83fba149b1bab6519ce3e32127
Quelldatensatz
uspto-grants-1999_01
Patentnummer
US05859063

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