Sodium Carbonate → 6-Hydroxyisochromen-1-one

HRID 1887543노트

반응식

HRID 1887543 반응식
B(Br)(Br)Br.C[O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[O:12][CH:11]=[CH:10]2.C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[OH:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][CH:16]=1)[C:13](=[O:17])[O:12][CH:11]=[CH:10]2

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 25134Boron tribromideHCID 151110126-Methoxyisochromen-1-one

생성물 1

HCID 668796996-Hydroxyisochromen-1-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of boron tribromide (1M in dichloromethane, 130 mL) was added to a solution of 6-methoxyisochromen-1-one (9.3 g) in dichloromethane (300 mL) at 0° C., and the mixture was stirred at room temperature for 16 h. After addition of sodium carbonate solution, the mixture was washed with ethyl acetate, and the aqueous phase was acidified with 2N HCl, extracted with ethyl acetate, dried over magnesium sulfate and concentrated. The residue was chromatographed on silica gel. The product with the molecular weight of 162.15 (C9H6O3) was obtained in this way; MS (ESI): 163 (M+H+).

후처리

  1. washthe mixture was washed with ethyl acetate
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel
  6. customThe product with the molecular weight of 162.15 (C9H6O3) was obtained in this way

출처 및 근거

ORD 기록
ord-c321b0fc29ad4f77a92afee44f02fb25
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08501771B2

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