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1-Bromopropane → HCID 15027467、化合物

HRID 1650888
ノート
印刷プレビュー

反応式

HRID 1650888 の反応式
[Mg].[CH3:2][CH2:3][CH2:4]Br.[OH:6][C:7]1[CH:20]=[CH:19][CH:18]=[CH:17][C:8]=1[C:9](=[O:16])[CH2:10][N:11]1[CH:15]=[CH:14][N:13]=[CH:12]1.[Cl-].[NH4+]>O1CCCC1>[OH:16][C:9]([C:8]1[CH:17]=[CH:18][CH:19]=[CH:20][C:7]=1[OH:6])([CH2:2][CH2:3][CH3:4])[CH2:10][N:11]1[CH:15]=[CH:14][N:13]=[CH:12]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 78401-BromopropaneHCID 25517Ammonium ChlorideHCID 4122933Ethanone, 1-(2-hydroxyphenyl)-2-(1H-imidazol-1-yl)-HCID 5462224Magnesium

生成物 1

HCID 15027467HCID 15027467、化合物収率 29%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a tetrahydrofuran solution of Grignard reagent prepared from 73 mg of magnesium and 369 mg of n-propyl bromide, 202 mg of 1-(2-hydroxyphenacyl) imidazole (II) was added dropwise under ice-cooled conditions while stirring, and the mixture was refluxed for 2 hours. After ice-cooling, an aqueous solution of ammonium chloride was added to the mixture to decompose the surplus amount of the Grignard reagent and addition salts produced in the reaction. Extraction with chloroform was performed on this mixture and the chloroform layer was washed with water, followed by drying over anhydrous magnesium sulfate. The extract thus obtained was purified by means of silica gel column chromatography (eluent: chloroform) to produce 70 mg of the title compound at a yield of 29%.

後処理

  1. additionwas added dropwise under ice-
  2. temperaturecooled conditions
  3. temperaturethe mixture was refluxed for 2 hours
  4. temperatureAfter ice-cooling
  5. customproduced in the reaction
  6. extractionExtraction with chloroform
  7. washthe chloroform layer was washed with water
  8. dry with materialby drying over anhydrous magnesium sulfate
  9. extractionThe extract thus
  10. customobtained
  11. customwas purified by means of silica gel column chromatography (eluent: chloroform)

出典と根拠

ORDレコード
ord-f4c849310bf747ff932bcabd58a2aff4
出典データセット
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04925953

反応ノート

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