Hydrochloric Acid → HCID 54396324、化合物

HRID 1076322ノート

反応式

HRID 1076322 の反応式
[H-].[Na+].[C:3]1([CH2:9][C:10](=[O:12])[CH3:11])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH3:13][C:14]1[CH:23]=[CH:22][C:17]([CH:18]=[CH:19][CH2:20]Br)=[CH:16][CH:15]=1.Cl.S([O-])([O-])(=O)=O.[NH4+].[NH4+]>C(COC)OC.O>[C:3]1([CH:9]([CH2:20][CH:19]=[CH:18][C:17]2[CH:22]=[CH:23][C:14]([CH3:13])=[CH:15][CH:16]=2)[C:10](=[O:12])[CH3:11])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 7678PhenylacetoneHCID 24758Sodium hydrideHCID 6097028Ammonium SulfateHCID 545379811-(3-Bromoprop-1-en-1-yl)-4-methylbenzene

生成物 1

HCID 54396324HCID 54396324、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 80711,2-Dimethoxyethane溶媒3 回

実験手順

Sodium hydride (6 g., 0.14 mole, oil dispersion) is suspended in glyme (200 ml.) and phenyl acetone (19.2 g., 0.14 mole) in glyme (50 ml.) is added dropwise with stirring. After complete addition the mixture is heated to reflux for 0.5 hour. The mixture is cooled in a cold water bath and a solution of p-methylcinnamyl bromide (32.2 g., 0.14 mole) in glyme (50 ml.) is added dropwise. When addition is complete, the mixture is refluxed for 18 hours then allowed to cool. Cold water (1000 ml.) is added and the mixture acidified with dilute hydrochloric acid. The mixture is saturated with ammonium sulfate and the organic material is extracted into ether. The extracts are washed with water, saturated brine, and dried (MgSO4). Filtration and removal of solvent in vacuo produces the crude product as a dark oil.

後処理

  1. additionAfter complete addition the mixture
  2. temperatureis heated
  3. temperatureto reflux for 0.5 hour
  4. temperatureThe mixture is cooled in a cold water bath
  5. additionWhen addition
  6. temperaturethe mixture is refluxed for 18 hours
  7. temperatureto cool
  8. extractionthe organic material is extracted into ether
  9. washThe extracts are washed with water, saturated brine
  10. dry with materialdried (MgSO4)
  11. filtrationFiltration and removal of solvent in vacuo

出典と根拠

ORDレコード
ord-0e21ba2fcbfe4a5f92046419282f017f
出典データセット
uspto-grants-1976_05
特許番号
US03956374

反応ノート

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