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Hydrochloric Acid → HCID 20150296、化合物

HRID 568340
ノート
印刷プレビュー

反応式

HRID 568340 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

10

反応物 4

HCID 313Hydrochloric Acid3 回HCID 10340Sodium CarbonateHCID 24489Sodium DithioniteHCID 20150314HCID 20150314、化合物

生成物 1

HCID 20150296HCID 20150296、化合物収率 10%

試薬・触媒・溶媒 5

HCID 702Ethanol溶媒
HCID 962
Water
溶媒
HCID 3283Diethyl Ether溶媒
HCID 3776Isopropanol溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-126ffc3651404930a0e9ed8dc9d1b96d
出典データセット
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04728647

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート