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

HRID 1200214ノート

反応式

HRID 1200214 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-4e3206e858e94f27b4dfe44e3c914694
出典データセット
uspto-grants-1990_02
特許番号
US04904775

反応ノート

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