Reaktion #163634

Reaktionsgleichung

3-chlorobenzohydrazide

pyridine

3-nitrobenzoyl chloride

→

N′1-(3-chlorobenzoyl)-3-nitrobenzene-1-carbohydrazide

Lösungsmittel

CH2Cl2

CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITat room temperature for overnight
2. 2
   EinengenThe resulting solution was concentrated
3. 3
   workup.ADDITIONdiluted with water
4. 4
   Filtrationthe solid was filtered
5. 5
   Waschenwashed with water
6. 6
   Sonstigedried

Vorschrift

To a solution of 3-chlorobenzohydrazide (1 equivalent) and pyridine (2 equivalents) in CH2Cl2 at 0° C. was added a CH2Cl2 solution of 3-nitrobenzoyl chloride (1 equivalents) and stirred at 0° C. for 1 h and then at room temperature for overnight. The resulting solution was concentrated and diluted with water, basified with NaHCO3, the solid was filtered, washed with water, dried and analyzed to obtain N′1-(3-chlorobenzoyl)-3-nitrobenzene-1-carbohydrazide. 1H NMR (DMSO-d6): δ 10.99 (s, 1H), 10.79 (s, 1H), 8.73 (bs, 1H), 8.43 (bdd, 1H, J=1.2 and 8.1 Hz), 8.33 (bdd, 1J, J=8.4 Hz), 7.95 (s, 1H), 7.87 (m, 2H), 7.67 (bdd, 1H, J=1.2 and 8.1 Hz), 7.57 (t, 1H, J=7.8 Hz); LCMS: purity: 85%; MS (m/e): 320 (MH+).

Quelle