Benzene → 3-Methyl-indan-1-one

HRID 511952

반응식

HRID 511952 반응식
[C:1](O)(=[O:5])/[CH:2]=[CH:3]/[CH3:4].[Al+3].[Cl-].[Cl-].[Cl-].[CH:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>>[CH3:4][CH:3]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:1](=[O:5])[CH2:2]1

참가 물질

4

반응물 3

HCID 241BenzeneHCID 637090Crotonic AcidHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 2595603-Methyl-indan-1-one

실험 절차

A solution of crotonic acid (20 g, 0.232 moles) in benzene (147 ml) was added AlCl3 (93 g, 0.748 moles) and the mixture was refluxed for 7 hours. Completion of the reaction was monitored by HPLC & GC. Excess benzene was distilled off and the reaction mixture was poured slowly into ice cold HCl. The organic compound was extracted with ethylacetate. The organic phase was washed thoroughly with water, dried, and evaporated under vacuum. The resultant oil was purified by high vacuum distillation (90-94° C. at ˜2 mm) giving 25 g (74%) of 99.2% pure 3-methyl-indan-1-one.

후처리

  1. temperaturethe mixture was refluxed for 7 hours
  2. distillationExcess benzene was distilled off
  3. additionthe reaction mixture was poured slowly into ice cold HCl
  4. extractionThe organic compound was extracted with ethylacetate
  5. washThe organic phase was washed thoroughly with water
  6. customdried
  7. customevaporated under vacuum
  8. distillationThe resultant oil was purified by high vacuum distillation (90-94° C. at ˜2 mm)

출처 및 근거

ORD 기록
ord-264733fe67cc40f589c5486f3f557ab2
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09102598B2

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