Potassium Hydroxide → 1-Methyl-5-(3-cyclohexylcarbonylpropyl)thio-1,2,3,4-tetrazole

HRID 1758311ノート

反応式

HRID 1758311 の反応式
[CH3:1][N:2]1[C:6](Cl)=[N:5][N:4]=[N:3]1.[CH:8]1([C:14]([CH2:16][CH2:17][CH2:18][SH:19])=[O:15])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.[OH-].[K+]>CO>[CH3:1][N:2]1[C:6]([S:19][CH2:18][CH2:17][CH2:16][C:14]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)=[O:15])=[N:5][N:4]=[N:3]1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 205098305-chloro-1-methyl-1H-1,2,3,4-tetrazoleHCID 205098493-Mercaptopropyl cyclohexyl ketone

生成物 1

HCID 130916241-Methyl-5-(3-cyclohexylcarbonylpropyl)thio-1,2,3,4-tetrazole収率 21.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1-Methyl-5-chloro-1,2,3,4-tetrazole (1.4 g) and 3-mercaptopropyl cyclohexyl ketone (1.9 g) are dissolved in methanol (50 ml) and potassium hydroxide (0.8 g) is added to the solution. The mixture is refluxed for 5 hours. Methanol is distilled off and water is added to the residue. The mixture is extracted with chloroform. The chloroform solution is washed with dil. aqueous sodium hydroxide, water and saturated aqueous sodium chloride and dried over sodium sulfate. Chloroform is distilled off and the residue is purified by column chromatography (Wakogel C-200, eluant: chloroform) to obtain 1-methyl-5-(3-cyclohexylcarbonylpropyl)thio-1,2,3,4-tetrazole (0.6 g) as colorless liquid, nD12 =1.5267.

後処理

  1. temperatureThe mixture is refluxed for 5 hours
  2. distillationMethanol is distilled off
  3. additionwater is added to the residue
  4. extractionThe mixture is extracted with chloroform
  5. washThe chloroform solution is washed with dil. aqueous sodium hydroxide, water and saturated aqueous sodium chloride
  6. dry with materialdried over sodium sulfate
  7. distillationChloroform is distilled off
  8. customthe residue is purified by column chromatography (Wakogel C-200, eluant: chloroform)

出典と根拠

ORDレコード
ord-f0ca18c9cd37484ab18f0e83a24459db
出典データセット
uspto-grants-1983_02
特許番号
US04372953

反応ノート

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