반응 #1242082

반응 방정식

methyl 2-chloroacetate

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

acetonitrile

→

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

반응 조건

후처리

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

실험 절차

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##

출처