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Hydrochloric Acid → HCID 20150296, 화합물

HRID 568340
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HRID 568340 반응식
[N+:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[C:9]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH:8]=[C:7]2[O:20][CH2:21][C:22]([N:24]1[CH2:29][CH2:28][O:27][CH2:26][CH2:25]1)=[O:23])([O-])=O.S(S([O-])=O)([O-])=O.[Na+].[Na+].Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.O.C(OCC)C.C(O)(C)C.C(OCC)(=O)C>[NH2:1][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[N:10]=[C:9]([C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[CH:8]=[C:7]2[O:20][CH2:21][C:22]([N:24]1[CH2:25][CH2:26][O:27][CH2:28][CH2:29]1)=[O:23]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 4

HCID 313Hydrochloric Acid3회HCID 10340Sodium CarbonateHCID 24489Sodium DithioniteHCID 20150314HCID 20150314, 화합물

생성물 1

HCID 20150296HCID 20150296, 화합물수율 10%

시약·촉매·용매 5

HCID 702Ethanol용매
HCID 962
Water
용매
HCID 3283Diethyl Ether용매
HCID 3776Isopropanol용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
20 °C

실험 절차

4-[(6-Nitro-2-phenyl-4-quinolyl)oxyacetyl]morpholine (12.5 g) in ethanol (550 cc) is heated under reflux for 10 minutes and a solution of sodium dithionite (27.7 g) in water (277 cc) is added in the course of 25 minutes. The mixture is cooled to room temperature (approximately 20° C.) and the ethanol removed under reduced pressure. The aqueous phase is stirred with ethyl acetate and the organic phase is washed with water, dried over magnesium sulphate and evaporated under reduced pressure. The residue obtained is taken up in ethyl ether and converted to the crude hydrochloride by adding a solution of hydrochloric acid in isopropanol. The hydrochloride is taken up with ethyl acetate and aqueous sodium carbonate solution. The precipitate which separates is filtered, heated for 25 minutes in refluxing ethyl acetate, filtered off and dried. 4-[(6-Amino-2-phenyl-4-quinolyl)oxyacetyl]morpholine (1.15 g), m.p. 194° C., is thereby isolated.

후처리

  1. temperatureunder reflux for 10 minutes
  2. customthe ethanol removed under reduced pressure
  3. washthe organic phase is washed with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated under reduced pressure
  6. customThe residue obtained
  7. filtrationThe precipitate which separates is filtered
  8. temperatureheated for 25 minutes
  9. temperaturein refluxing ethyl acetate
  10. filtrationfiltered off
  11. customdried

출처 및 근거

ORD 기록
ord-126ffc3651404930a0e9ed8dc9d1b96d
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04728647

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