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Chloroacetone → 2-Propanone, 1-((1-methyl-1H-tetrazol-5-yl)thio)-

HRID 1758302
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HRID 1758302 반응식
[CH3:1][N:2]1[C:6]([SH:7])=[N:5][N:4]=[N:3]1.C(=O)([O-])[O-].[K+].[K+].[CH3:14][C:15]([CH2:17]Cl)=[O:16]>CC(C)=O>[CH3:1][N:2]1[C:6]([S:7][CH2:14][C:15](=[O:16])[CH3:17])=[N:5][N:4]=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 178482017HCID 178482017, 화합물

생성물 1

HCID 30619772-Propanone, 1-((1-methyl-1H-tetrazol-5-yl)thio)-수율 48%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

1-Methyl-5-mercapto-1,2,3,4-tetrazole (0.01 mol), potassium carbonate (0.015 mol) and α-chloroacetone (0.015 mol) are added to acetone (50 ml) and the mixture is refluxed with stirring for 2 hours. The reaction mixture is concentrated to dryness under reduced pressure and the residue is dissolved in chloroform. Insolubles are filtered off. The filtrate is concentrated under reduced pressure and the residue is purified by silica gel column chromatography [Kieselgel 60, eluant: benzene-ether (10:1)] and the product is recrystallized from methanol-ether to obtain 1-methyl-5-acetylmethylthio-1,2,3,4-tetrazole (yield 48%) as colorless needles, m.p. 31° C.

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후처리

  1. temperaturethe mixture is refluxed
  2. concentrationThe reaction mixture is concentrated to dryness under reduced pressure
  3. dissolutionthe residue is dissolved in chloroform
  4. filtrationInsolubles are filtered off
  5. concentrationThe filtrate is concentrated under reduced pressure
  6. customthe residue is purified by silica gel column chromatography [Kieselgel 60, eluant: benzene-ether (10:1)]
  7. customthe product is recrystallized from methanol-ether

출처 및 근거

ORD 기록
ord-251cd1ba05c642a9817e905ef8c3e208
출처 데이터셋
uspto-grants-1983_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04372953

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