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

HRID 2234236

反応式

HRID 2234236 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-eeb1a068930844398b12dcfc3cf9e695
出典データセット
uspto-grants-2010_05
特許番号
US07709664B2

関連ノート

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