Ammonia → HCID 178492429, Verbindung

HRID 2075946Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2075946
[CH2:1]([O:8][C:9]1[C:18]([O:19][CH3:20])=[CH:17][C:12]([C:13](Cl)=[N:14][OH:15])=[C:11]([I:21])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[N:23](C)C=O.N.C(OCC)(=O)C>O>[CH2:1]([O:8][C:9]1[C:18]([O:19][CH3:20])=[CH:17][C:12]([C:13]([NH:14][OH:15])=[NH:23])=[C:11]([I:21])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

6

Edukt 4

HCID 222AmmoniaHCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 866472264-benzyloxy-N-hydroxy-2-iodo-5-methoxy-benzimidoylchloride

Produkt 1

HCID 178492429HCID 178492429, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

To a mixture of 4-benzyloxy-N-hydroxy-2-iodo-5-methoxy-benzimidoylchloride and N,N-dimethylformamide (110 mL) was added a 28% ammonia in water (12 mL) under ice-bath cooling. After stirring for 3 hours under ice-bath cooling, water and ethyl acetate were added to the mixture. The separated organic layer was washed with water and brine successively, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was triturated with hexane:diethyl ether=1:4 to give the title compound (9.3 g).

Aufarbeitung

  1. temperaturecooling
  2. temperaturecooling
  3. washThe separated organic layer was washed with water and brine successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was triturated with hexane

Quellen und Nachweise

ORD-Eintrag
ord-0aa487be90be4afebf7bf65fe3b0e39d
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07923462B2

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