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

HRID 1758302
ノート
印刷プレビュー

反応式

HRID 1758302 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 178482017HCID 178482017、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-251cd1ba05c642a9817e905ef8c3e208
出典データセット
uspto-grants-1983_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04372953

反応ノート

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