2,2',4,4'-Tetrahydroxybenzophenone → 3,6-dihydroxy-9H-xanthen-9-one

HRID 54714

反応式

HRID 54714 の反応式
O[C:2]1[CH:17]=[C:16]([OH:18])[CH:15]=[CH:14][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][C:7]=1[OH:13])=[O:5]>O>[OH:18][C:16]1[CH:17]=[CH:2][C:3]2[C:4](=[O:5])[C:6]3[C:7]([O:13][C:14]=2[CH:15]=1)=[CH:8][C:9]([OH:12])=[CH:10][CH:11]=3

参加物

3

反応物 1

HCID 85712,2',4,4'-Tetrahydroxybenzophenone

生成物 1

HCID 57493223,6-dihydroxy-9H-xanthen-9-one収率 92.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2,2',4,4'-Tetrahydroxybenzophenone (2.5 g, 10.15 mmol.) was heated in 20 ml of water at 195°-200° C. for 4 hours (Aldrich pressure tube). After cooling, the crude product was filtered off and mixed with 25 ml of water. The resulting suspension was refluxed for 25 min. and filtered at about 60° C. Pure product 3,6-dihydroxyxanthone 2.15 g was obtained in 90.4% yield. It did not melt below 330° C. HNMR (DMSO): 10.780 (s,2H), 7.983 (d,2H,J=8.6 Hz), 6,822 (m,4H). MS: 228,220, 1717, 115, 100, 69, 63.

後処理

  1. temperatureAfter cooling
  2. filtrationthe crude product was filtered off
  3. additionmixed with 25 ml of water
  4. temperatureThe resulting suspension was refluxed for 25 min.
  5. filtrationfiltered at about 60° C

出典と根拠

ORDレコード
ord-d7202d4f58c54fdcb377034cbd137134
出典データセット
uspto-grants-1997_04
特許番号
US05623080

関連ノート

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