Sodium Iodide → N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)-2-morpholinoacetamide

HRID 1958882Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1958882
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:10]=[CH:9][N:8]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[C:13]([Cl:18])[CH:12]=2)[N:7]=1)=[O:4].[NH:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O>[Cl:18][C:13]1[CH:12]=[C:11]([N:8]2[CH:9]=[CH:10][C:6]([NH:5][C:3](=[O:4])[CH2:2][N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)=[N:7]2)[CH:16]=[CH:15][C:14]=1[Cl:17]

Komponenten

6

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A mixture of 2-chloro-N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)acetamide (0.22 g, 0.74 mmol), morpholine (71 mg, 0.81 mmol), potassium carbonate (0.22 g, 1.62 mmol) and sodium iodide (0.11 g, 0.74 mmol) in dry dimethylformamide (5 ml) was stirred and warmed at 100° C., overnight, in a dry nitrogen atmosphere. The solvent was evaporated in vacuo and water was added to the crude residue. The dark solid precipitated was filtered and dried yielding a crude product purified by crystallization in ethyl acetate, and 0.23 g of N-(1-(3,4-dichlorophenyl)-1H-pyrazol-3-yl)-2-morpholinoacetamide was obtained as a beige colour solid with m.p.=125-127° C.

Aufarbeitung

  1. customThe solvent was evaporated in vacuo and water
  2. additionwas added to the crude residue
  3. customThe dark solid precipitated
  4. filtrationwas filtered
  5. customdried
  6. customyielding a crude product
  7. custompurified by crystallization in ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-52f897bef7384d609ac7015eafa40d33
Quelldatensatz
uspto-grants-2013_04
Patentnummer
US08410159B2

Notizen zur Reaktion

Wird geladen…