Lawesson's reagent → 4-Morpholinobenzenecarbothioamide

HRID 56115

Reaktionsgleichung

Reaktionsgleichung von HRID 56115
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:15]=[CH:14][C:10]([C:11]([NH2:13])=O)=[CH:9][CH:8]=2)[CH2:3][CH2:2]1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:25])=CC=1>C1COCC1>[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:15]=[CH:14][C:10]([C:11](=[S:25])[NH2:13])=[CH:9][CH:8]=2)[CH2:3][CH2:2]1

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 221422424-(Morpholin-4-yl)benzamide

Produkt 1

HCID 27953604-MorpholinobenzenecarbothioamideAusbeute 83,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

To a solution of 4-morpholinobenzamide (4.91 g, 23.80 mmol) in THF (70 mL) was added Lawesson's Reagent (10.60 g, 26.20 mmol) with stirring. The mixture was heated at 70° C. for 4 h, then cooled to rt and concentrated in vacuo. CH2Cl2 (30 mL) and water (100 mL) was added to the residue. The mixture was then filtered and the filter cake was washed with water and dried to give the title compound as a yellow solid (4.41 g, 83.3%).

Aufarbeitung

  1. temperaturecooled to rt
  2. concentrationconcentrated in vacuo
  3. additionCH2Cl2 (30 mL) and water (100 mL) was added to the residue
  4. filtrationThe mixture was then filtered
  5. washthe filter cake was washed with water
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-b3263675a8b3462c97d4844f0524773b
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09434695B2

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