5-Acetamido-4-hydroxy-5,6,7,8-tetrahydroquinoline-3-carboxylic Acid Ethyl Ester → HCID 178474099、化合物

HRID 1680536ノート

反応式

HRID 1680536 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][C:9]2[CH2:10][CH2:11][CH2:12][CH:13]([NH:17][C:18](=[O:20])[CH3:19])[C:14]=2[C:15]=1[OH:16])=[O:5])C>[OH-].[Na+]>[C:18]([NH:17][CH:13]1[CH2:12][CH2:11][CH2:10][C:9]2[N:8]=[CH:7][C:6]([C:4]([OH:5])=[O:3])=[C:15]([OH:16])[C:14]1=2)(=[O:20])[CH3:19]

参加物

3

反応物 1

HCID 1784694745-Acetamido-4-hydroxy-5,6,7,8-tetrahydroquinoline-3-carboxylic Acid Ethyl Ester

生成物 1

HCID 178474099HCID 178474099、化合物収率 55.6%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
110 °C

実験手順

5-Acetamido-4-hydroxy-5,6,7,8-tetrahydroquinoline-3-carboxylic acid ethyl ester (0.8 g) was suspended in 20 ml of 1 N sodium hydroxide. The resulting reaction mixture was heated on an oil bath at 110° C. for 2 hours. After being cooled, the reaction mixture was filtered to remove the insoluble matter, and the filtrate was adjusted to pH 2.5 with dilute hydrochloric acid. The precipitate so formed was separated by filtration to obtain a yield of 0.4 g of the desired compound. This compound melted (and decomposed) at 285°-287° C. (uncorrected values). Its infrared absorption spectrum (KBr tablet) had absorption peaks at 3420, 3340, 3260, 3080, 2940, 1710, 1650, 1635, 1290, and 810 cm-1. and its n.m.r. spectrum (CF3COOH, 60Mc, TMS) had signals at δ values of 1.8-2.6 (4H, m), 2.43 (3H, s), 2.9-3.5 (2H, m), 5.72 (1H, d, J=8.3 Hz), 8.47 (1H, d, J=8.3 Hz), and 9.0-9.3 (1H, m).

後処理

  1. customThe resulting reaction mixture
  2. temperatureAfter being cooled
  3. filtrationthe reaction mixture was filtered
  4. customto remove the insoluble matter
  5. customThe precipitate so formed
  6. customwas separated by filtration

出典と根拠

ORDレコード
ord-e505b4261c8042528c51e43653403644
出典データセット
uspto-grants-1981_06
特許番号
US04273932

反応ノート

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