Chloroacetone → 4,6-Dimethyl-7-acetonyloxycoumarin

HRID 1646425ノート

反応式

HRID 1646425 の反応式
[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([OH:13])=[C:9]([CH3:12])[CH:10]=2)[O:5][C:4](=[O:14])[CH:3]=1.C([O-])([O-])=O.[K+].[K+].Cl[CH2:22][C:23](=[O:25])[CH3:24]>CC(C)=O>[CH3:1][C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:13][CH2:22][C:23]([CH3:24])=[O:25])=[C:9]([CH3:12])[CH:10]=2)[O:5][C:4](=[O:14])[CH:3]=1

参加物

5

反応物 3

HCID 6571ChloroacetoneHCID 11430Potassium CarbonateHCID 107977397-Hydroxy-4,6-dimethyl-2H-1-benzopyran-2-one

生成物 1

HCID 545237254,6-Dimethyl-7-acetonyloxycoumarin

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 4,6-dimethyl-7-hydroxycoumarin (III) (5.0 g), anhydrous K2CO3 (10 g), chloroacetone (2.5 ml) and acetone (150 ml) was refluxed for 12 h under stirring. From the refluxed mixture the solid was filtered and washed several times with acetone. The acetonic solution and the pooled washings were concentrated to dryness and the residue crystallized from MeOH, yielding 4,6-dimethyl-7-acetonyloxycoumarin (XXXVII) (5.1 g; m.p. 190° C.) ##STR42##

後処理

  1. temperaturewas refluxed for 12 h
  2. filtrationFrom the refluxed mixture the solid was filtered
  3. washwashed several times with acetone
  4. concentrationThe acetonic solution and the pooled washings were concentrated to dryness
  5. customthe residue crystallized from MeOH

出典と根拠

ORDレコード
ord-066564c5ac8b4bfbaff2caa5d36ec86d
出典データセット
uspto-grants-1993_01
特許番号
US05179217

反応ノート

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