Ammonium Chloride → HCID 22063451、化合物

HRID 506550ノート

反応式

HRID 506550 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10](=[O:12])[CH3:11])=[CH:5][CH:4]=1)[CH3:2].[CH3:13][Mg]Br.[Cl-].[NH4+]>C(OCC)C>[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([CH3:13])([OH:12])[CH3:11])=[CH:5][CH:4]=1)[CH3:2]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 70192734-EthylphenylacetoneHCID 178418573HCID 178418573、化合物

生成物 1

HCID 22063451HCID 22063451、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

14.8 g (90 mmol) of 1-(4-ethylphenyl)propan-2-one dissolved in diethyl ether is added dropwise to 39 mL of a 3 molar solution of methylmagnesium bromide in diethyl ether while being cooled with an ice bath in such a way that the temperature does not exceed 30° C. After the addition has ended, the reaction mixture is refluxed for 1.5 hours and then hydrolyzed with 10% ammonium chloride solution. After the removal of the organic phase, the aqueous phase is extracted with diethyl ether. The combined ether phases are washed with water, dried with sodium sulfate, and evaporated down. The oil thus obtained is further reacted directly. Yield: 15.5 g (90%).

後処理

  1. temperaturewhile being cooled with an ice bath in such a way that the temperature
  2. customdoes not exceed 30° C
  3. additionAfter the addition
  4. temperaturethe reaction mixture is refluxed for 1.5 hours
  5. customAfter the removal of the organic phase
  6. extractionthe aqueous phase is extracted with diethyl ether
  7. washThe combined ether phases are washed with water
  8. dry with materialdried with sodium sulfate
  9. customevaporated down
  10. customThe oil thus obtained
  11. customis further reacted directly

出典と根拠

ORDレコード
ord-16d1fa1c00544d73b350983fdb98bec5
出典データセット
uspto-grants-2010_08
特許番号
US07786111B2

反応ノート

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