Hydrochloric Acid → [2-(2-Thienyl)ethylamino](2-chlorophenyl)acetamide hydrochloride

HRID 323885Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 323885
C(OC)(=[O:3])C.Cl.[S:7]1[CH:11]=[CH:10][CH:9]=[C:8]1[CH2:12][CH2:13][NH:14][CH:15]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[Cl:24])[C:16]#[N:17].CO>>[ClH:24].[S:7]1[CH:11]=[CH:10][CH:9]=[C:8]1[CH2:12][CH2:13][NH:14][CH:15]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[Cl:24])[C:16]([NH2:17])=[O:3]

Komponenten

5

Edukt 4

HCID 313Hydrochloric Acid2×HCID 887MethanolHCID 6584Methyl AcetateHCID 10858772[2-(2-Thienyl)ethylamino](2-chlorophenyl)acetonitrile

Produkt 1

HCID 21953219[2-(2-Thienyl)ethylamino](2-chlorophenyl)acetamide hydrochloride

Reaktionsbedingungen

Temperatur
22.5 °C

Versuchsvorschrift

Into 1200 ml of methyl acetate 204 g (5.6 mol) of hydrogen chloride gas is introduced at 15-25° C., and to the solution 221.4 g (0.8 mol) of the [2-(2-thienyl)ethylamino](2-chlorophenyl)acetonitrile of formula (I), prepared as described in Example 1., and 48 ml (1.2 mol) of methanol are added and the mixture is stirred at 20-25° C. for 6 hours. In the course of the reaction first the hydrochloride of the starting “nitrile”, then gradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals. The crystals are collected by filtration, washed with methyl acetate and dried. Weight: 249 g (94%) mp.: 231-232° C.

Aufarbeitung

  1. customgradually the hydrochloride of the resulting “acid amide” precipitates, in the form of white crystals
  2. filtrationThe crystals are collected by filtration
  3. washwashed with methyl acetate
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-f4a7dd8fee7148799c35afe14e004dcf
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06215005B1

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