Reaktion #49951

ord-4ace12a6e29447b3bbd6b021605bd28a

Reaktionsgleichung

CC(C)(C)NN.Cl
t-butyl hydrazine hydrochloride
Cc1ccccc1
toluene
O=C(Cl)C1C=c2ccc3cccc4ccc(c2c43)C1=O
pyrenonecarbonyl chloride
CCOCC
ether
CCCCCC
hexane
Cc1cccc(C(=O)N(NC(=O)C2C=c3ccc4cccc5ccc(c3c54)C2=O)C(C)(C)C)c1
N'-t-butyl-N-pyrenonecarbonyl-N'-(3-toluoyl)hydrazine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationthe solid product was filtered
  2. 2
    Waschenwashed with water
  3. 3
    workup.STIRRINGThe solid product (0.5 g) was stirred in toluene (10 ml)
  4. 4
    workup.ADDITIONaqueous sodium hydroxide and m-toluoyl chloride (0.8 g) was added dropwise
  5. 5
    workup.STIRRINGAfter stirring for 5 hours
  6. 6
    workup.ADDITIONhexane and ether were added
  7. 7
    Filtrationthe solid product filtered
  8. 8
    Sonstigeair dried

Vorschrift

To a stirred suspension of t-butyl hydrazine hydrochloride (0.02 mol) in toluene (20 ml) and aqueous hydroxide (5 ml of 50% solution) at room temperature was added pyrenonecarbonyl chloride (0.01 mol). After stirring the reaction mixture for 20 minutes, ether and hexane were added and the solid product was filtered and washed with water. The solid product (0.5 g) was stirred in toluene (10 ml) and aqueous sodium hydroxide and m-toluoyl chloride (0.8 g) was added dropwise. After stirring for 5 hours, hexane and ether were added and the solid product filtered and air dried.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424333uspto-grants-1995_06