5-Fluorobenzene-1,3-diol → Umbelliferone

HRID 253720

反応式

HRID 253720 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-Fluorobenzene-1,3-diol

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-6b3dab5e691549ec9674ed348d6cad28
出典データセット
uspto-grants-2011_01
特許番号
US07872142B2

関連ノート

読み込み中…