Potassium Hydroxide → N-(2-morpholinophenyl)cyanamide

HRID 1492277Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1492277
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[NH:13][C:14]([NH2:16])=S)[CH2:3][CH2:2]1.[OH-].[K+].O.O.O.C([O-])(=O)C.[Pb+2].C([O-])(=O)C>O>[O:1]1[CH2:2][CH2:3][N:4]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[NH:13][C:14]#[N:16])[CH2:5][CH2:6]1

Komponenten

5

Edukt 3

HCID 14797Potassium HydroxideHCID 22456Lead diacetate trihydrateHCID 27411931-(2-Morpholinophenyl)thiourea

Produkt 1

HCID 15746517N-(2-morpholinophenyl)cyanamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

1-(2-morpholinophenyl)thiourea (10.6 g) was suspended in boiling water (80 ml) and a solution of potassium hydroxide (25.2 g) in hot water (70 ml) was added. The mixture was heated to 90° C. and aliquot portions of a hot solution of lead acetate trihydrate (17.5 g) in water (80 ml) added and the mixture heated under reflux for 10 minutes and cooled to ambient temperature. The mixture was filtered and the filtrate acidified with acetic acid to pH 6. The solid which formed was separated by filtration, washed with water and recrystallised from ethylacetate to give N-(2-morpholinophenyl)cyanamide (m.p. 175°-176° C.).

Aufarbeitung

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 10 minutes
  3. temperaturecooled to ambient temperature
  4. filtrationThe mixture was filtered
  5. customThe solid which formed
  6. customwas separated by filtration
  7. washwashed with water
  8. customrecrystallised from ethylacetate

Quellen und Nachweise

ORD-Eintrag
ord-d957ba0cc2704dbcaa2affdfdf0bde80
Quelldatensatz
uspto-grants-1994_12
Patentnummer
US05373008

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