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

HRID 54714

반응식

HRID 54714 반응식
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

참가 물질

3

반응물 1

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

생성물 1

HCID 57493223,6-dihydroxy-9H-xanthen-9-one수율 92.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d7202d4f58c54fdcb377034cbd137134
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05623080

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