Water → 4-Chloro-N'-(diphenylmethylene)butanehydrazide

HRID 8204

Reaktionsgleichung

Reaktionsgleichung von HRID 8204
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].[C:8](=[N:21][NH2:22])([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.N1C=CC=CC=1.O>ClCCl>[C:8](=[N:21][NH:22][C:5](=[O:6])[CH2:4][CH2:3][CH2:2][Cl:1])([C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 1049PyridineHCID 783704-Chlorobutyryl chlorideHCID 79304Diphenylmethylidenehydrazine

Produkt 1

HCID 3198334-Chloro-N'-(diphenylmethylene)butanehydrazide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

4-Chlorobutyryl chloride (57 mL, 510 mmol) is added to a solution of benzophenone hydrazone (100 g, 510 mmol) and pyridine (41 mL, 510 mmol) in anhydrous dichloromethane (520 mL) under nitrogen at a rate that maintains a gentle reflux throughout the addition. The mixture is stirred for 0.5 h and poured into water (1 L). The layers are separated and the organic layer washed with brine, dried (sodium sulfate), filtered, and concentrated in vacuo to yield 4-chloro-butyric acid benzhydrylidene-hydrazide as a residue.

Aufarbeitung

  1. temperaturea gentle reflux throughout the addition
  2. customThe layers are separated
  3. washthe organic layer washed with brine
  4. dry with materialdried (sodium sulfate)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-6e9f813cdbf440e28165af869bd6f9f1
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07087626B2

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