N'-Benzylidene-4-methylbenzene-1-sulfonohydrazide → Benzene, (diazomethyl)-

HRID 428440Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 428440
S([NH:11][N:12]=[CH:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)(C1C=CC(C)=CC=1)(=O)=O.C[O-].[Na+]>CO>[C:14]1([CH:13]=[N+:12]=[N-:11])[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1

Komponenten

4

Edukt 2

HCID 277551N'-Benzylidene-4-methylbenzene-1-sulfonohydrazideHCID 10942334Sodium Methoxide

Produkt 1

HCID 136601Benzene, (diazomethyl)-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

In an oven-dried round bottom flask was placed benzaldehyde tosylhydrazone (1.15 g, 4.2 mmol), followed by 4.3 mL of a 1.0 M solution of sodium methoxide in methanol (2.3 g Na metal dissolved in absolute methanol and diluted to 100 mL). The mixture was swirled until all the contents dissolved. Most of the solvent was removed via rotary evaporation and the last traces of solvent by evacuation of the flask under high vacuum for 2 hours. The solid obtained was subjected to a Kugelrohr distillation at 215° C. and 200 millitorr for 1 hour. At 68-70° C., the title compound, as a red oil, was collected in a receiver flask in a quantitative yield.

Aufarbeitung

  1. customIn an oven-dried round bottom flask was placed
  2. dissolutiondissolved
  3. customMost of the solvent was removed via rotary evaporation
  4. customThe solid obtained
  5. distillationwas subjected to a Kugelrohr distillation at 215° C.
  6. wait200 millitorr for 1 hour
  7. customAt 68-70° C., the title compound, as a red oil, was collected in a receiver flask in a quantitative yield

Quellen und Nachweise

ORD-Eintrag
ord-7d1b90adda91403ca5d87e3b3516a405
Quelldatensatz
uspto-grants-2001_11
Patentnummer
US06313290B1

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