Diethylamine → N,N-diethyl-4-iodobenzamide

HRID 747109

Reaktionsgleichung

Reaktionsgleichung von HRID 747109
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[CH3:11][CH2:12][N:13](CC)[CH2:14][CH3:15].N(CC)CC>C(Cl)Cl>[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([N:13]([CH2:14][CH3:15])[CH2:12][CH3:11])=[O:7])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 8021DiethylamineHCID 8471TriethylamineHCID 743734-Iodobenzoyl chloride

Produkt 1

HCID 875218N,N-diethyl-4-iodobenzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a mixture of 4-iodo-benzoyl chloride (75 g) in 500 mL CH2Cl2 was added a mixture of Et3N (50 mL) and Et2NH (100 mL) at 0° C. After the addition, the resulting reaction mixture was warmed up to room temperature in 1 hr and was then washed with saturated ammonium chloride. The organic extract was dried (Na2SO4), filtered and concentrated. Residue was recrystallized from hot hexanes to give 80 g of INTERMEDIATE 5.

Aufarbeitung

  1. additionwas added
  2. additionAfter the addition
  3. customthe resulting reaction mixture
  4. washwas then washed with saturated ammonium chloride
  5. extractionThe organic extract
  6. dry with materialwas dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customResidue was recrystallized from hot hexanes

Quellen und Nachweise

ORD-Eintrag
ord-28b78c804afd448ea22a9636a4b3cf3b
Quelldatensatz
uspto-grants-2008_07
Patentnummer
US07396834B2

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