Sodium Carbonate → 6-Hydroxyisochromen-1-one

HRID 1887543ノート

反応式

HRID 1887543 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 668796996-Hydroxyisochromen-1-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-c321b0fc29ad4f77a92afee44f02fb25
出典データセット
uspto-grants-2013_08
特許番号
US08501771B2

反応ノート

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