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1(3H)-Isobenzofuranone, 3-hydroxy-7-methoxy- → HCID 16748834, 화합물

HRID 22172
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인쇄 미리보기

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HRID 22172 반응식
[OH:1][CH:2]1[C:11]2[C:6](=[C:7]([O:12]C)[CH:8]=[CH:9][CH:10]=2)[C:4](=[O:5])[O:3]1.[Cl-].[Cl-].[Cl-].[Al+3]>C(Cl)Cl>[OH:1][CH:2]1[C:11]2[C:6](=[C:7]([OH:12])[CH:8]=[CH:9][CH:10]=2)[C:4](=[O:5])[O:3]1
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참가 물질

4

반응물 2

HCID 27525831(3H)-Isobenzofuranone, 3-hydroxy-7-methoxy-HCID 6451240Aluminum(III) Chloride

생성물 1

HCID 16748834HCID 16748834, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
27 °C

실험 절차

3.0 g of 3-hydroxy-7-methoxy-phthalide ]see B. L. Chenard et al., J. Org. Chem. 49, 318 (1984)] are introduced in portions into a suspension of 8.2 g of aluminium trichloride in 50 ml of methylene chloride, the internal temperature being maintained at 27° C. The mixture is stirred at room temperature for a further 5 hours, is then poured into 200 ml of ice-cold 1N hydrochloric acid and extracted three times with 200 ml of ethyl acetate each time. The organic solution is washed with sodium chloride solution and dried over anhydrous magnesium sulfate. Evaporation of the solvent and recrystallisation from ethyl acetate and n-hexane yield pure 3,7-dihydroxyphthalide, m.p. 124°-126° C.

후처리

  1. extractionextracted three times with 200 ml of ethyl acetate each time
  2. washThe organic solution is washed with sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customEvaporation of the solvent and recrystallisation from ethyl acetate and n-hexane

출처 및 근거

ORD 기록
ord-2eb9932e21774af2b0a27f1f00230fb5
출처 데이터셋
uspto-grants-1995_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05428002

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