beta,beta'-Thiodipropionitrile → 3-cinnamoylamino-4-(2'-cyano-4',6'-dinitrophenylazo)-N,N-diethylaniline

HRID 1704200

Reaktionsgleichung

[C:1](CCSCCC#N)#[N:2].[C:10]([NH:20][C:21]1[CH:22]=[C:23]([CH:29]=[CH:30][C:31]=1[N:32]=[N:33][C:34]1[C:39]([N+:40]([O-:42])=[O:41])=[CH:38][C:37]([N+:43]([O-:45])=[O:44])=[CH:36][C:35]=1Br)[N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])(=[O:19])[CH:11]=[CH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[C-]#N.[Na+]>O>[C:10]([NH:20][C:21]1[CH:22]=[C:23]([CH:29]=[CH:30][C:31]=1[N:32]=[N:33][C:34]1[C:39]([N+:40]([O-:42])=[O:41])=[CH:38][C:37]([N+:43]([O-:45])=[O:44])=[CH:36][C:35]=1[C:1]#[N:2])[N:24]([CH2:27][CH3:28])[CH2:25][CH3:26])(=[O:19])[CH:11]=[CH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

Komponenten

Reaktionsbedingungen

Temperatur: 100 °C

Versuchsvorschrift

Into a solution composed of 6.8 parts of cuprous bromide in 300 parts by volume of bis-(β-cyanoethyl) sulfide, there are introduced 26 parts of 3-cinnamoylamino-4-(2'-bromo-4', 6'-dinitrophenylazo)-N,N-diethylaniline. The mixture is heated to 100° C. and, during several minutes, a solution of 2.6 parts of sodium cyanide in 16 parts of water is allowed to flow in. Stirring is continued for 1 to 2 hours more, at 115° C. After cooling to 30° C., the 3-cinnamoylamino-4-(2'-cyano-4',6'-dinitrophenylazo)-N,N-diethylaniline formed is separated, under the same conditions as in example 1. The yield is 85.5%.

Aufarbeitung

customat 115° C
temperatureAfter cooling to 30° C.

Quellen und Nachweise

ORD-Eintrag: ord-1875c55deca343338b28bab2887ad01d
Quelldatensatz: uspto-grants-1978_11
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04126610

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