2-Cyanoethanethioamide → HCID 178458231, Verbindung

HRID 2362823Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2362823
[Si:1]([O:8][CH:9]([CH3:20])[CH2:10][O:11][C:12]1[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[C:21]([CH2:23][C:24]([NH2:26])=[S:25])#[N:22]>C(O)C>[NH2:26][C:24]1[C:23]([C:21]#[N:22])=[C:16]([C:15]2[CH:18]=[CH:19][C:12]([O:11][CH2:10][CH:9]([O:8][Si:1]([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2])[CH3:20])=[CH:13][CH:14]=2)[C:23]([C:21]#[N:22])=[C:24]([SH:25])[N:26]=1

Komponenten

4

Edukt 2

HCID 14162772-CyanoethanethioamideHCID 592019704-(2-{[tert-Butyl(dimethyl)silyl]oxy}propoxy)benzaldehyde

Produkt 1

HCID 178458231HCID 178458231, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 1.77 g (5.99 mmol) of the compound from Example 41A and 1.26 g (12.59 mmol) of cyanothioacetamide in 25 ml of ethanol is stirred at +78° C. for 6 h. The mixture is then cooled to RT and stirred at this temperature for a further 20 h. The resulting precipitate is filtered off with suction and washed with cold diethyl ether. Further product is obtained from the concentrated filtrate solution by chromatographic purification on silica gel 60 (mobile phase gradient cyclohexane/ethyl acetate 1:1→1:4).

Aufarbeitung

  1. filtrationThe resulting precipitate is filtered off with suction
  2. washwashed with cold diethyl ether
  3. customFurther product is obtained from the concentrated filtrate solution by chromatographic purification on silica gel 60 (mobile phase gradient cyclohexane/ethyl acetate 1:1→1:4)

Quellen und Nachweise

ORD-Eintrag
ord-e6df32c03e6e4fce828a081cf8247103
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08691850B2

Notizen zur Reaktion

Wird geladen…