Sulfuric Acid → 3-benzyl-6,7-dihydroxy-4-methyl-2H-chromen-2-one

HRID 1595135

反応式

HRID 1595135 の反応式
C([O:4][C:5]1[CH:10]=CC(OC(=O)C)=[CH:7][C:6]=1[O:15]C(=O)C)(=O)C.[CH2:19]([CH:26]([C:32]([CH3:34])=O)[C:27]([O:29][CH2:30][CH3:31])=[O:28])[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.S(=O)(=O)(O)O>>[OH:4][C:5]1[CH:10]=[C:31]2[C:30](=[CH:7][C:6]=1[OH:15])[O:29][C:27](=[O:28])[C:26]([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[C:32]2[CH3:34]

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 691691,2,4-TriacetoxybenzeneHCID 246929Ethyl alpha-benzylacetoacetate

生成物 1

HCID 163946973-benzyl-6,7-dihydroxy-4-methyl-2H-chromen-2-one

実験手順

1,2,4-triacetoxybenzene (6.3 g, 25 mmol) and ethyl 2-benzylacetoacetate (5.5 g, 25 mmol) were heated together as described in Example 1. 75% sulphuric acid (35 ml) was added to the stirred solution and stirring continued for 16 hours. The dark coloured suspension was poured into ice/water (350 ml) with good stirring and the grey suspension filtered and the residue washed with abundant water. The residual solid was air dried and recrystallised from hot ethanol with subsequent addition of a little water to aid crystallization. The esculetin derivative formed small white needles (5.5 g, 75.3%).

後処理

  1. stirringwith good stirring
  2. filtrationthe grey suspension filtered
  3. washthe residue washed with abundant water
  4. customdried
  5. customrecrystallised from hot ethanol with subsequent addition of a little water
  6. customcrystallization

出典と根拠

ORDレコード
ord-9fd58c97fca9431ba35debecc4e8df3d
出典データセット
uspto-grants-2001_09
特許番号
US06287798B1

関連ノート

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