Acetic Acid → 5H-indeno[5,6-d][1,3]dioxole

HRID 1195269노트

반응식

HRID 1195269 반응식
O[CH:2]1[C:10]2[C:5](=[CH:6][C:7]3[O:13][CH2:12][O:11][C:8]=3[CH:9]=2)[CH2:4][CH2:3]1.C(O)(=O)C.O.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1>[CH2:12]1[O:11][C:8]2[CH:9]=[C:10]3[C:5]([CH:4]=[CH:3][CH2:2]3)=[CH:6][C:7]=2[O:13]1

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 11430Potassium CarbonateHCID 14514900HCID 14514900, 화합물

생성물 1

HCID 190016835H-indeno[5,6-d][1,3]dioxole수율 92.7%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 10.8 g of 1-hydroxy-5,6-methylenedioxyindane and 15 ml of acetic acid in 100 ml of toluene was heated under reflux for 4 h. Water and a small amount of potassium carbonate were added to the reaction mixture. After extraction with ethyl acetate, the organic layer was washed with water and an aqueous common salt solution and dried over magnesium sulfate. The solvent was distilled off and the residue was treated according to silica gel column chromatography (chloroform/hexane=1:3) to obtain 9.0 g of the intended compound in the form of colorless crystals.

후처리

  1. temperatureunder reflux for 4 h
  2. extractionAfter extraction with ethyl acetate
  3. washthe organic layer was washed with water
  4. dry with materialan aqueous common salt solution and dried over magnesium sulfate
  5. distillationThe solvent was distilled off
  6. additionthe residue was treated

출처 및 근거

ORD 기록
ord-ed6bbbf5fddd443998b5d023fc0e6336
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05110956

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