Imidazole → HCID 20291998、化合物

HRID 262778ノート

反応式

HRID 262778 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[O:6]([CH2:13][CH2:14][N:15]([CH2:19][CH2:20][CH3:21])[C:16](Cl)=[O:17])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>O1CCCC1>[O:6]([CH2:13][CH2:14][N:15]([CH2:19][CH2:20][CH3:21])[C:16]([N:1]1[CH:5]=[CH:4][N:3]=[CH:2]1)=[O:17])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 795ImidazoleHCID 12238093Carbamic chloride, (2-phenoxyethyl)propyl-

生成物 1

HCID 20291998HCID 20291998、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 75 ml. dry tetrahydrofuran were added 6.8 g. imidazole and 12.075 g. N-2-phenoxyethyl-N-propylcarbamoyl chloride. The reactants were boiled together under reflux for twenty-four hours, cooled to room temperature and filtered to remove imidazole hydrochloride. The solvent was then removed by evaporation from the steam bath, the last traces being removed under vacuum. An oily residue remained which was extracted into ether, washed with water, dried over anhydrous sodium sulphate, the solvent removed and the residual oil distilled under vacuum, to give 1-(N-2-phenoxyethyl-N-propylcarbamoyl) imidazole, boiling point 209° C./1.0 mm.

後処理

  1. temperatureunder reflux for twenty-four hours
  2. filtrationfiltered
  3. customto remove imidazole hydrochloride
  4. customThe solvent was then removed by evaporation from the steam bath
  5. customthe last traces being removed under vacuum
  6. extractionwas extracted into ether
  7. washwashed with water
  8. dry with materialdried over anhydrous sodium sulphate
  9. customthe solvent removed
  10. distillationthe residual oil distilled under vacuum

出典と根拠

ORDレコード
ord-fca818c79e7643699932fc15cb3aed60
出典データセット
uspto-grants-1979_05
特許番号
US04154945

反応ノート

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