Chloromethyl Methyl Ether → N-methoxymethyl-N'-t-butyl-N,N'-dibenzoylhydrazine

HRID 21630

Reaktionsgleichung

Reaktionsgleichung von HRID 21630
[C:1]([N:5]([C:15](=[O:22])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[NH:6][C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:23][O:24][CH2:25]Cl>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH3:23][O:24][CH2:25][N:6]([C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[N:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[C:15](=[O:22])[C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1

Komponenten

5

Edukt 2

HCID 7864Chloromethyl Methyl EtherHCID 863071,2-Dibenzoyl-1-(tert-butyl)hydrazine

Produkt 1

HCID 15294609N-methoxymethyl-N'-t-butyl-N,N'-dibenzoylhydrazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 94433Tetrabutylammonium hydrogen sulfateKatalysatorHCID 1140TolueneLösungsmittel

Versuchsvorschrift

N'-t-butyl-N,N'-dibenzoylhydrazine (2 g, 0.007M) was stirred at room temperature in a two phase system of toluene-50% sodium hydroxide with 100 mg of phase transfer catalyst (tetra-n-butylammonium hydrogen sulfate). Methoxymethyl chloride (1.2 g, 0.015M) was added dropwise and the mixture was stirred 3 hours. The layers were separated and the toluene layer was washed several times with water (until the water washes were neutral). The toluene solution was dried over anhydrous magnesium sulfate and the toluene removed under vacuum to afford N-methoxymethyl-N'-t-butyl-N,N'-dibenzoylhydrazine as a thick oil.

Aufarbeitung

  1. customThe layers were separated
  2. washthe toluene layer was washed several times with water (until the water washes
  3. dry with materialThe toluene solution was dried over anhydrous magnesium sulfate
  4. customthe toluene removed under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-7d2cb3f08be145dbb405d7662fdadc8f
Quelldatensatz
uspto-grants-1995_06
Patentnummer
US05424333

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