Salicylic Acid → 1,3-Dihydroxy-xanthone

HRID 83092

反応式

HRID 83092 の反応式
[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

参加物

3

反応物 2

HCID 338Salicylic AcidHCID 359Phloroglucinol

生成物 1

HCID 54881931,3-Dihydroxy-xanthone収率 93.4%

反応条件

温度
80 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-d4c5ccb4eec247519b3c0bf411d20f5b
出典データセット
uspto-grants-2014_09
特許番号
US08846749B2

関連ノート

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