Phosgene → HCID 13742718, Verbindung

HRID 1733143Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1733143
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:6]=1[C:7]#[N:8].[C:13](Cl)(Cl)=[O:14].C[C@H]1CO[C@@]2(O[C@H]3C[C@H]4[C@@H]5CC=C6C[C@@H](O)CC[C@]6(C)[C@H]5CC[C@]4(C)[C@H]3[C@@H]2C)CC1>ClC1C=CC=CC=1>[C:7]([C:6]1[C:5]([C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][S:3][C:2]=1[N:1]=[C:13]=[O:14])#[N:8]

Komponenten

5

Edukt 3

HCID 6371Phosgene3×HCID 99474DiosgeninHCID 5968662-Amino-4-(1,1-dimethylethyl)-3-thiophenecarbonitrile

Produkt 1

HCID 13742718HCID 13742718, VerbindungAusbeute 60,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7964ChlorobenzeneLösungsmittel2×

Versuchsvorschrift

A solution of 90 g (0.5 mole) of 2-amino-3-cyano-4-tert.-butyl-thiophene in 300 ml of chlorobenzene was added dropwise to a solution of 150 g of phosgene in 1.5 liters of chlorobenzene at 0°-5° C. Thereafter, the mixture was slowly heated to the boil, while passing further phosgene in, and excess phosgene was then driven off by passing dry nitrogen in. For working up, the solvent was stripped off under reduced pressure and the residue was distilled. 62 g of 3-cyano-4-tert.-butyl-thien-2-yl isocyanate, which boiled at 163° C. under a pressure of 20 mm Hg, were obtained in this manner.

Aufarbeitung

  1. temperatureThereafter, the mixture was slowly heated to the boil
  2. distillationthe residue was distilled

Quellen und Nachweise

ORD-Eintrag
ord-24e22ecf6aa34398bd29d444aced0dc2
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04240820

Notizen zur Reaktion

Wird geladen…