Dimethylcarbamoyl Chloride → 1H-1,2,4-Triazole-1-carboxamide, 3-tert-butyl-N,N-dimethyl-5-(methylthio)-

HRID 1833561ノート

反応式

HRID 1833561 の反応式
[C:1]([C:5]1[NH:9][C:8]([S:10][CH3:11])=[N:7][N:6]=1)([CH3:4])([CH3:3])[CH3:2].[CH3:12][N:13]([CH3:17])[C:14](Cl)=[O:15]>N1C=CC=CC=1>[CH3:12][N:13]([CH3:17])[C:14]([N:7]1[C:8]([S:10][CH3:11])=[N:9][C:5]([C:1]([CH3:4])([CH3:2])[CH3:3])=[N:6]1)=[O:15]

参加物

4

反応物 2

HCID 6598Dimethylcarbamoyl ChlorideHCID 178503613HCID 178503613、化合物

生成物 1

HCID 30492461H-1,2,4-Triazole-1-carboxamide, 3-tert-butyl-N,N-dimethyl-5-(methylthio)-

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 57.6 g (0.338 mol) of 3-tert.butyl-5-methylthio-4H-1,2,4-triazole and 38g (0.355 mol) of dimethylcarbamyl chloride in 300 ml of pyridine was maintained at reflux temperature for 16 hrs. After the pyridine was removed at reduced pressure on the rotary evaporator, water was added followed by chloroform. The organic layer was washed with successive portions of dilute hydrochloric acid, water and brine then dried over Na2SO4. The solvent was removed in vacuo to give 75 g, nD26 1.5165 of an oil. Spectral properties agree with the structure

後処理

  1. temperatureat reflux temperature for 16 hrs
  2. customAfter the pyridine was removed at reduced pressure on the rotary evaporator, water
  3. additionwas added
  4. washThe organic layer was washed with successive portions of dilute hydrochloric acid, water and brine
  5. dry with materialthen dried over Na2SO4
  6. customThe solvent was removed in vacuo
  7. customto give 75 g

出典と根拠

ORDレコード
ord-529082be42b9413abc067bead47ce636
出典データセット
uspto-grants-1978_01
特許番号
US04066774

反応ノート

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