Hydrochloric Acid → 3-hydroxy-N-(2-hydroxyphenyl)benzamide

HRID 1883697

反応式

HRID 1883697 の反応式
C[O:2][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[O:15]C)=[O:7].Cl.N1C=CC=CC=1.Cl>>[OH:2][C:3]1[CH:4]=[C:5]([CH:17]=[CH:18][CH:19]=1)[C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[OH:15])=[O:7]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 9028663-methoxy-N-(2-methoxyphenyl)benzamideHCID 10176127Pyridinium chloride

生成物 1

HCID 235084853-hydroxy-N-(2-hydroxyphenyl)benzamide収率 27.1%

反応条件

温度
190 °C

実験手順

451 mg of 3-methoxy-N-(2-methoxyphenyl)benzamide and 1.58 g of pyridine hydrochloride were mixed, and stirred on an oil bath at 190° C. for 2 hours. After cooling, dilute hydrochloric acid was added to the reaction mixture, and the product was extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium hydrogen carbonate and dried over anhydrous sodium sulfate. After the solvent was distilled oft the resulting crude product was recrystallized from methanol to obtain 109 mg of 3-hydroxy-N-(2-hydroxyphenyl)benzamide.

後処理

  1. temperatureAfter cooling
  2. extractionthe product was extracted with ethyl acetate
  3. washThe extract was washed with a saturated aqueous solution of sodium hydrogen carbonate
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationAfter the solvent was distilled oft the resulting crude product
  6. customwas recrystallized from methanol

出典と根拠

ORDレコード
ord-6e4d1a4308d040539db3d1486d9713c0
出典データセット
uspto-grants-2004_07
特許番号
US06762205B1

関連ノート

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