3-Anilinopropionitrile → N-(2-cyanoethyl)-carbanilic acid-[3-(cyclopropylcarbonylamino)-phenyl]-ester

HRID 67033

Reaktionsgleichung

Reaktionsgleichung von HRID 67033
[C:1]([CH2:3][CH2:4][NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)#[N:2].[CH:12]1([C:15]([NH:17][C:18]2[CH:19]=[C:20]([O:24][C:25](Cl)=[O:26])[CH:21]=[CH:22][CH:23]=2)=[O:16])[CH2:14][CH2:13]1>C(#N)C>[CH:12]1([C:15]([NH:17][C:18]2[CH:19]=[C:20]([O:24][C:25](=[O:26])[N:5]([CH2:4][CH2:3][C:1]#[N:2])[C:6]3[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=3)[CH:21]=[CH:22][CH:23]=2)=[O:16])[CH2:13][CH2:14]1

Komponenten

4

Edukt 2

HCID 141003-AnilinopropionitrileHCID 54149755Chloroformic acid-[3-(cyclopropylcarbonylamino)-phenyl]-ester

Produkt 1

HCID 20455829N-(2-cyanoethyl)-carbanilic acid-[3-(cyclopropylcarbonylamino)-phenyl]-ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

29.2 g N-(2-cyanoethyl)-aniline is dissolved in 200 ml acetonitrile and then reacted with 23.97 g chloroformic acid-[3-(cyclopropylcarbonylamino)-phenyl]-ester with stirring, with which the temperature of the solution rises to about 35° C. After standing overnight the solvent is removed under vacuum, The remaining oily residue is treated with water, the water is decanted and the oil brought to crystallization with a 1:1 mixture of isopropyl ether/isopropanol. The crystallizate is finally recrystallized from isopropanol.

Aufarbeitung

  1. customrises to about 35° C
  2. customthe solvent is removed under vacuum
  3. additionThe remaining oily residue is treated with water
  4. customthe water is decanted
  5. customthe oil brought to crystallization with a 1:1 mixture of isopropyl ether/isopropanol
  6. customThe crystallizate is finally recrystallized from isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-54e76b6ffa0e4c9681bc432320543779
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04344790

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