Sodium Iodide → 2,3-dihydro-2,4,6-trimethyl-7-hydroxy-2-benzyl-1H-indene-1-one

HRID 4999노트

반응식

HRID 4999 반응식
[CH3:1][C:2]1([CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:10][C:9]2[C:4](=[C:5]([O:13]C)[C:6]([CH3:12])=[CH:7][C:8]=2[CH3:11])[C:3]1=[O:15].[I-].[Na+].[Cl-].[Al+3].[Cl-].[Cl-]>C(#N)C>[CH3:1][C:2]1([CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH2:10][C:9]2[C:4](=[C:5]([OH:13])[C:6]([CH3:12])=[CH:7][C:8]=2[CH3:11])[C:3]1=[O:15]

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 6451240Aluminum(III) ChlorideHCID 148347342,3-dihydro-2,4,6-trimethyl-7-methoxy-2-benzyl-1H-inden-1-one

생성물 1

HCID 143905432,3-dihydro-2,4,6-trimethyl-7-hydroxy-2-benzyl-1H-indene-1-one

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

23.0 Grams of 2,3-dihydro-2,4,6-trimethyl-7-methoxy-2-benzyl-1H-inden-1-one and 25.8 g of sodium iodide were dissolved in 90 ml of acetonitrile. To this solution was added 22.9 g of aluminium chloride at room temperature and stirred for 1 hour. Then the solvent was removed by evaporation under a reduced pressure, and the residue thus obtained was extracted with ethyl acetate. The extract was washed with an aqueous solution saturated with sodium chloride, an aqueous solution of sodium thiosulfate and an aqueous solution saturated with sodium chloride in this order, and the insoluble matters were removed by filtration. The solvent was removed by evaporation and the residue thus obtained was recrystallized from n-hexane to obtain 19.7 of 2,3-dihydro-2,4,6-trimethyl-7-hydroxy-2-benzyl-1H-indene-1-one. Colorless prism-like crystals.

후처리

  1. customThen the solvent was removed by evaporation under a reduced pressure
  2. customthe residue thus obtained
  3. extractionwas extracted with ethyl acetate
  4. washThe extract was washed with an aqueous solution saturated with sodium chloride
  5. customan aqueous solution of sodium thiosulfate and an aqueous solution saturated with sodium chloride in this order, and the insoluble matters were removed by filtration
  6. customThe solvent was removed by evaporation
  7. customthe residue thus obtained
  8. customwas recrystallized from n-hexane

출처 및 근거

ORD 기록
ord-adac67716cd442838e451fe27a615b95
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05242919

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