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5-(4-methoxybenzoyl)-6-methyl-2(1H)-pyridinone → 5-(4-hydroxybenzoyl)-6-methyl-2(1H)-pyridinone

HRID 638198
ノート
印刷プレビュー

反応式

HRID 638198 の反応式
C[O:2][C:3]1[CH:18]=[CH:17][C:6]([C:7]([C:9]2[CH:10]=[CH:11][C:12](=[O:16])[NH:13][C:14]=2[CH3:15])=[O:8])=[CH:5][CH:4]=1>Br>[OH:2][C:3]1[CH:4]=[CH:5][C:6]([C:7]([C:9]2[CH:10]=[CH:11][C:12](=[O:16])[NH:13][C:14]=2[CH3:15])=[O:8])=[CH:17][CH:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 217799405-(4-methoxybenzoyl)-6-methyl-2(1H)-pyridinone

生成物 1

HCID 202536305-(4-hydroxybenzoyl)-6-methyl-2(1H)-pyridinone収率 93.1%

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

実験手順

A mixture containing 13 g of 5-(4-methoxybenzoyl)-6-methyl-2(1H)-pyridinone and 100 ml of 48% aqueous hydrogen bromide solution was refluxed for 7 hours and then allowed to stand at room temperature overnight. The reaction mixture was concentrated to dryness on a rotary evaporator. To the residue was added 100 ml of water and the aqueous mixture was neutralized by adding aqueous ammonium hydroxide solution. The solid was collected, washed with water and air dried. The solid was recrystallized from 100 ml of ethanol and dried at 80°-85° C. to yield 11.4 g of 5-(4-hydroxybenzoyl)-6-methyl-2(1H)-pyridinone, m.p. 280°-282° C.

後処理

  1. temperaturewas refluxed for 7 hours
  2. concentrationThe reaction mixture was concentrated to dryness on a rotary evaporator
  3. additionTo the residue was added 100 ml of water
  4. additionby adding aqueous ammonium hydroxide solution
  5. customThe solid was collected
  6. washwashed with water and air
  7. customdried
  8. customThe solid was recrystallized from 100 ml of ethanol
  9. customdried at 80°-85° C.

出典と根拠

ORDレコード
ord-fa57b6e213484d2ebf0a7cfefa7d9fbf
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04560691

反応ノート

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