Sulfuric Acid → 7-Hydroxy-4,6-dimethyl-2H-1-benzopyran-2-one

HRID 359496

反応式

HRID 359496 の反応式
[OH:1][C:2]1C=C(O)[CH:5]=[CH:4][C:3]=1[CH3:9].OS(O)(=O)=O.[CH2:15]([O:17][C:18](=[O:23])[CH2:19][C:20]([CH3:22])=O)[CH3:16]>>[CH3:22][C:20]1[C:5]2[C:15](=[CH:16][C:2]([OH:1])=[C:3]([CH3:9])[CH:4]=2)[O:17][C:18](=[O:23])[CH:19]=1

参加物

4

反応物 3

HCID 1118Sulfuric AcidHCID 8868Ethyl AcetoacetateHCID 103331,3-Benzenediol, 4-methyl-

生成物 1

HCID 107977397-Hydroxy-4,6-dimethyl-2H-1-benzopyran-2-one

実験手順

A solution of 2,4-dihydroxytoluene (10.0 g) in ethylacetoacetate (12 ml) was poured in small portion into conc. H2SO4 (26 ml), chilling in an ice bath. After the addition was completed the solid obtained was separated by filtration, washed several times with water up to neutrality of the washings, dried and crystallized from MeOH, yielding 4,6-dimethyl-7-hydroxycoumarin (III) (10.64 g; m.p. 273° C.). ##STR9##

後処理

  1. temperaturechilling in an ice bath
  2. additionAfter the addition
  3. customobtained
  4. customwas separated by filtration
  5. washwashed several times with water up to neutrality of the washings
  6. customdried
  7. customcrystallized from MeOH

出典と根拠

ORDレコード
ord-d9d006fbc7f34f76bf56b49995c94735
出典データセット
uspto-grants-1991_03
特許番号
US05001147

関連ノート

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