Sodium Bicarbonate → HCID 12769827、化合物

HRID 26685

反応式

HRID 26685 の反応式
[CH2:1]([C:3]1[O:4][C:5]2[CH:14]=[CH:13][C:12]([CH:15]([CH3:20])[C:16]([O:18]C)=[O:17])=[CH:11][C:6]=2[C:7](=[O:10])[C:8]=1[CH3:9])[CH3:2].C(=O)(O)[O-].[Na+]>C(O)C.O>[CH2:1]([C:3]1[O:4][C:5]2[CH:14]=[CH:13][C:12]([CH:15]([CH3:20])[C:16]([OH:18])=[O:17])=[CH:11][C:6]=2[C:7](=[O:10])[C:8]=1[CH3:9])[CH3:2]

参加物

5

反応物 2

HCID 516892Sodium BicarbonateHCID 21322008Methyl 2-[2-ethyl-3-methyl-4-oxo-4H-1-benzopyran-6-yl]propionate

生成物 1

HCID 12769827HCID 12769827、化合物収率 42.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

A solution of methyl 2-(2-ethyl-3-methyl-4-oxo-4H-1-benzopyran-6-yl)propionate (1 g) in ethanol (120 mls), and sodium bicarbonate (1 g) in water (30 mls) was refluxed for 20 hours. The ethanol was removed on a `Rotavapor` and the residue was washed with ether (3×50 mls). After acidification with dilute hydrochloric acid, the aqueous phase was extracted with ethyl acetate (3×50 mls), which was washed with brine solution (3×30 mls), dried over anhydrous magnesium sulphate and evaporated to yield an off-white solid. This was recrystallised from ethyl acetate to yield the product as a pale yellow solid (0.4 g; 42%), mp 196°-198° C.

後処理

  1. customThe ethanol was removed on a `Rotavapor` and the residue
  2. washwas washed with ether (3×50 mls)
  3. extractionAfter acidification with dilute hydrochloric acid, the aqueous phase was extracted with ethyl acetate (3×50 mls), which
  4. washwas washed with brine solution (3×30 mls)
  5. dry with materialdried over anhydrous magnesium sulphate
  6. customevaporated
  7. customto yield an off-white solid
  8. customThis was recrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-0f9ad95629134fd6a655ea057ec27db2
出典データセット
uspto-grants-1979_04
特許番号
US04151179

関連ノート

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