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

HRID 1680536노트

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HRID 1680536 반응식
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]

참가 물질

3

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온도
110 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e505b4261c8042528c51e43653403644
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04273932

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