Potassium thiocyanate → 4-Tert-butyl-1,3-dihydroimidazole-2-thione

HRID 1579124ノート

反応式

HRID 1579124 の反応式
Cl.[NH2:2][CH2:3][C:4](=O)[C:5]([CH3:8])([CH3:7])[CH3:6].[S-:10][C:11]#[N:12].[K+]>O>[C:5]([C:4]1[N:12]=[C:11]([SH:10])[NH:2][CH:3]=1)([CH3:8])([CH3:7])[CH3:6]

参加物

4

反応物 2

HCID 516872Potassium thiocyanateHCID 221479671-Amino-3,3-dimethylbutan-2-one hydrochloride

生成物 1

HCID 1784413604-Tert-butyl-1,3-dihydroimidazole-2-thione

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

35.2 g. 1-Amino-3,3-dimethylbutan-2-one hydrochloride and 30 g. potassium thiocyanate in 50 ml. water was warmed on the steam bath for two hours. After cooling, the solid formed was collected, washed with water, dried and recrystallised from industrial methylated spirit to give 4-tert.butylimidazole-2-thiol, melting point 232°-234°C. A solution/suspension of this in industrial methylated spirit was added to a solution of 4.5 g. sodium hydroxide in 100 ml. water. 17.6 g. Ethyl iodide was added forming a lower layer and the mixture was shaken for two minutes whilst the ethyl iodide reacted and dispersed. After 20 minutes the alkali was neutralised by passing in carbon dioxide and the methylated spirit removed by evaporation. The solid was collected, washed with water, dried and on recrystallisation from toluene gave 2-ethylthio-4-tert.butylimidazole, melting point 116.5°-120°C.

後処理

  1. temperatureAfter cooling
  2. customthe solid formed
  3. customwas collected
  4. washwashed with water
  5. customdried
  6. customrecrystallised from industrial methylated spirit

出典と根拠

ORDレコード
ord-e1669dcd89734b3bbd568a990944d0e6
出典データセット
uspto-grants-1976_02
特許番号
US03940484

反応ノート

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