Salicylic Acid → 1,3-Dihydroxy-xanthone

HRID 83092

반응식

HRID 83092 반응식
[C:1](O)(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)O.[C:11]1([CH:19]=[C:17]([OH:18])[CH:16]=[C:14]([OH:15])[CH:13]=1)[OH:12]>>[OH:12][C:11]1[C:19]2[C:1](=[O:9])[C:2]3[C:8](=[CH:7][CH:6]=[CH:5][CH:3]=3)[O:18][C:17]=2[CH:16]=[C:14]([OH:15])[CH:13]=1

참가 물질

3

반응물 2

HCID 338Salicylic AcidHCID 359Phloroglucinol

생성물 1

HCID 54881931,3-Dihydroxy-xanthone수율 93.4%

반응 조건

온도
80 °C

실험 절차

Salicylic acid (1.25 g, 9.1 mmol), phloroglucinol (1.26 g, 10 mmol), ZnCl□(3.1 g, 22.8 mmol) and POCl□ (8 mL) were charged to a dry round-bottom flask, and the reaction mixture was stirred at 80° C. for 4 hours. After the reaction was completed, the reaction mixture was cooled to room temperature and was very slowly added to ice water. When the reaction liquid was poured in ice water, ice was added portionwise to prevent overheating. The resulting precipitate was allowed to stand at 4° C. overnight, combined, washed with water and ether, and then dried under reduced pressure to give a reddish brown solid compound (1.94 g, 93%).

후처리

  1. temperaturethe reaction mixture was cooled to room temperature
  2. customWhen the reaction liquid
  3. additionice was added portionwise
  4. waitto stand at 4° C. overnight
  5. washwashed with water and ether
  6. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-d4c5ccb4eec247519b3c0bf411d20f5b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846749B2

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