Sodium Hydroxide → 2,3-Quinolinedicarboxylic acid

HRID 542271

反応式

HRID 542271 の反応式
[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[C:3]([C:11]([O:13]CC)=[O:12])[C:2]=1[C:16]([O:18]CC)=[O:17].[OH-].[Na+]>C(O)C.O>[N:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[C:3]([C:11]([OH:13])=[O:12])[C:2]=1[C:16]([OH:18])=[O:17]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 10880272Diethyl 2,3-quinolinedicarboxylate

生成物 1

HCID 695082,3-Quinolinedicarboxylic acid

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of diethyl 2,3-quinolinedicarboxylate (0.162 mol) in ethanol (150 mL) is added a solution of sodium hydroxide (0.50 mol) in water (400 mL). The mixture is heated at reflux for five hours, and the ethanol then removed by distillation at atmospheric pressure. The solution is cooled in an ice bath, diluted with water (100 mL), and acidified with concentrated hydrochloric acid, added in small increments. The precipitate is filtered, washed with water, and air dried to afford the desired 2,3-quinolinedicarboxylic acid as the trihydrate; mp 271°-277° C.

後処理

  1. temperatureThe mixture is heated
  2. temperatureat reflux for five hours
  3. customthe ethanol then removed by distillation at atmospheric pressure
  4. temperatureThe solution is cooled in an ice bath
  5. additiondiluted with water (100 mL)
  6. additionadded in small increments
  7. filtrationThe precipitate is filtered
  8. washwashed with water, and air
  9. customdried

出典と根拠

ORDレコード
ord-82078cd114684e7c8d424ab1b33955cc
出典データセット
uspto-grants-1987_04
特許番号
US04656283

関連ノート

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