Ammonium Chloride → HCID 22063451, 화합물

HRID 506550노트

반응식

HRID 506550 반응식
[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]

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 70192734-EthylphenylacetoneHCID 178418573HCID 178418573, 화합물

생성물 1

HCID 22063451HCID 22063451, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-16d1fa1c00544d73b350983fdb98bec5
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786111B2

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