Sodium Hydroxide → 6,7-Dimethoxy-2,3-quinolinedicarboxylic acid

HRID 2248104ノート

反応式

HRID 2248104 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[C:8]([C:15]([O:17]CC)=[O:16])[C:7]([C:20]([O:22]CC)=[O:21])=[CH:6]2.[OH-].[Na+]>>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[N:9]=[C:8]([C:15]([OH:17])=[O:16])[C:7]([C:20]([OH:22])=[O:21])=[CH:6]2

参加物

3

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 133519282,3-Diethyl 6,7-dimethoxy-2,3-quinolinedicarboxylate

生成物 1

HCID 139230016,7-Dimethoxy-2,3-quinolinedicarboxylic acid収率 101%

実験手順

A suspension of 26.7 g (80 mmol) of 6,7-dimethoxy-2,3-quinolinedicarboxylic acid, diethyl ester, prepared as described by S. B. Kadin and C. H. Lamphere, J. Org. Chem., 49, 4999 (1984), in 10% sodium hydroxide solution (containing 16 g (400 mmol) of sodium hydroxide) was refluxed for 5 hours. After the filtration of the hot solution, 300 ml of water and subsequently 3N hydrochloric acid were added until the pH reached 1.0. The solids were filtered off by suction, washed thoroughly with water, and dried in vacuo to give 22.4 g of the desired product having a melting point of 264°-266° C.

後処理

  1. customprepared
  2. filtrationAfter the filtration of the hot solution, 300 ml of water and subsequently 3N hydrochloric acid
  3. additionwere added until the pH
  4. filtrationThe solids were filtered off by suction
  5. washwashed thoroughly with water
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-0a74dd49d3034eb28bde941251a4e7cf
出典データセット
uspto-grants-1991_08
特許番号
US05037983

反応ノート

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