4-Chlororesorcinol → 6-Chloro-7-hydroxy coumarin

HRID 1671491

反応式

HRID 1671491 の反応式
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([OH:6])=[CH:4][C:3]=1[OH:9].[CH2:10]([CH:17](C(C)=O)[C:18](OCC)=[O:19])C1C=CC=CC=1>OS(O)(=O)=O>[Cl:1][C:2]1[CH:8]=[C:7]2[C:5](=[CH:4][C:3]=1[OH:9])[O:6][C:18](=[O:19])[CH:17]=[CH:10]2

参加物

4

反応物 2

HCID 17314-ChlororesorcinolHCID 246929Ethyl alpha-benzylacetoacetate

生成物 1

HCID 53931666-Chloro-7-hydroxy coumarin収率 104.9%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

4-Chlororesorcinol (26.25 g, 0.182 mol) and ethyl 2-benzylacetoacetate (40 g, 0.182 mol) are mixed in 70% H2SO4 (350 mL) at 0° C. The reaction mixture is stirred at room temperature for 72 hours and poured into ice water. The solid is filtered and washed with water. The crude product is recrystallized from ethanol/chloroform to afford 6-chloro-7-hydroxy coumarin intermediate (37.52 g, 68.7%).

後処理

  1. filtrationThe solid is filtered
  2. washwashed with water
  3. customThe crude product is recrystallized from ethanol/chloroform

出典と根拠

ORDレコード
ord-b365926c56ad41a4b5dea9adf27d3d2b
出典データセット
uspto-grants-2011_08
特許番号
US07994318B2

関連ノート

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