5-Fluororesorcinol → Umbelliferone

HRID 1671494ノート

反応式

HRID 1671494 の反応式
F[C:2]1[CH:7]=[C:6]([OH:8])[CH:5]=[C:4]([OH:9])[CH:3]=1>S(=O)(=O)(O)O>[OH:9][C:4]1[CH:5]=[C:6]2[C:7]([CH:4]=[CH:5][C:6](=[O:8])[O:8]2)=[CH:2][CH:3]=1

参加物

3

反応物 1

HCID 126587785-Fluororesorcinol

生成物 1

HCID 5281426Umbelliferone収率 146.9%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

1-Fluoro-3,5-dihydroxybenzene (1.0 g, 7.8 mmol) and ethyl 2-benzyl acetoacetate (1.72 g, 7.8 mmol) are suspended in 20 mL of 70% sulfuric acid at room temperature. The reaction mixture is stirred for 24 hours and poured into ice water. The solid is filtered and washed with water. The yellowish crude product is re-crystallized from hot ethanol to afford the 7-hydroxy coumarin intermediate (929 mg, 42%).

後処理

  1. filtrationThe solid is filtered
  2. washwashed with water
  3. customThe yellowish crude product is re-crystallized from hot ethanol

出典と根拠

ORDレコード
ord-b699d2efe0e04786b171c1278f5726a9
出典データセット
uspto-grants-2011_08
特許番号
US07994318B2

反応ノート

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