Water → HCID 21412476, Verbindung

HRID 2071798Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2071798
[C:1](Cl)(=[O:3])[CH3:2].[CH3:5][O:6][C:7]([NH:9][C:10](=[S:27])[NH:11][C:12]1[CH:13]=[C:14]([CH:16]=[CH:17][C:18]=1[NH:19][C:20]([NH:22][C:23]([O:25][CH3:26])=[O:24])=[S:21])[NH2:15])=[O:8].C(=O)(O)[O-].[Na+].O>CC(C)=O>[C:1]([NH:15][C:14]1[CH:16]=[CH:17][C:18]([NH:19][C:20]([NH:22][C:23]([O:25][CH3:26])=[O:24])=[S:21])=[C:12]([NH:11][C:10]([NH:9][C:7]([O:6][CH3:5])=[O:8])=[S:27])[CH:13]=1)(=[O:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 516892Sodium BicarbonateHCID 21412481HCID 21412481, Verbindung

Produkt 1

HCID 21412476HCID 21412476, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

Acetyl chloride (1.66 g; 0.0212 mole) was added dropwise during five minutes to a stirred suspension of 3,4-bis-(3-methoxycarbonyl-2-thioureido)aniline (4.0 g; 0.0112 mole) and sodium bicarbonate (1.78 g; 0.0212 mole) in dry acetone (50 ml). The temperature of the reaction mixture rose spontaneously to 30° C. After completion of the addition, the mixture was refluxed with stirring for 6 hours, cooled and poured into water. The solid which separated was filtered off, washed well with water and crystallised from ethanol to give 4-acetamido-1,2-bis-(3-methoxycarbonyl-2-thioureido)benzene, m.p. 183°-185° C. (with decomposition).

Aufarbeitung

  1. customrose spontaneously to 30° C
  2. additionAfter completion of the addition
  3. temperaturethe mixture was refluxed
  4. temperaturecooled
  5. customThe solid which separated
  6. filtrationwas filtered off
  7. washwashed well with water
  8. customcrystallised from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-10bbc5fa083c4af69dbe8da209c8ec15
Quelldatensatz
uspto-grants-1977_09
Patentnummer
US04048326

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