Reaktion #1242082

Reaktionsgleichung

methyl 2-chloroacetate

thiocarbazic acid-O-(3,3,5-trimethylcyclohexyl)-ester

acetonitrile

→

3-(3,3,5-trimethylcyclohexyloxy)-5-methyl-4-methoxycarbonyl-pyrazole

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeobtained in this manner
2. 2
   workup.STIRRINGAfter stirring for 12 hours at room temperature
3. 3
   workup.ADDITIONthe mixture of solids which
4. 4
   Sonstigehas precipitated out
5. 5
   Sonstigeis separated by filtration
6. 6
   Waschenwashed with acetone
7. 7
   workup.STIRRINGThe solids mixture is then stirred into 200 ml of aqueous ammonia solution (12 wt%)
8. 8
   Extraktionsubsequently extracted twice with methylene chloride (150 ml each time)
9. 9
   TrocknenAfter the methylene chloride solution has been dried over sodium sulfate
10. 10
    Sonstigethe solvent is evaporated
11. 11
    Sonstigeafter recrystallization
12. 12
    workup.ADDITIONfrom a 2:1 mixture of toluene and n-hexane

Vorschrift

At room temperature and while stirring, 84 l g of methyl 2-chloroacetate is added to a solution, in 250 ml of acetonitrile, of the thiocarbazic acid-O-(3,3,5-trimethylcyclohexyl)-ester obtained in this manner. After stirring for 12 hours at room temperature, the mixture of solids which has precipitated out is separated by filtration and washed with acetone. The solids mixture is then stirred into 200 ml of aqueous ammonia solution (12 wt%) and subsequently extracted twice with methylene chloride (150 ml each time). After the methylene chloride solution has been dried over sodium sulfate, the solvent is evaporated. The solid which remains has, after recrystallization from a 2:1 mixture of toluene and n-hexane, a melting point of 167° to 168° C. and has, according to combustion analysis and nmr spectroscopy, the composition: ##STR11##

Quelle