Stannous Chloride → HCID 146733、化合物

HRID 1354567ノート

反応式

HRID 1354567 の反応式
[N+:1]([C:4]1[CH:25]=[CH:24][C:7]([CH:8]=[CH:9][C:10]2[C:11]3[C:16]([N:17]=[C:18]4[C:23]=2[CH:22]=[CH:21][CH:20]=[CH:19]4)=[CH:15][CH:14]=[CH:13][CH:12]=3)=[CH:6][CH:5]=1)([O-])=O.[Sn](Cl)Cl>C(OCC)(=O)C.C(O)C>[NH2:1][C:4]1[CH:25]=[CH:24][C:7]([CH:8]=[CH:9][C:10]2[C:23]3[C:18]([N:17]=[C:16]4[C:11]=2[CH:12]=[CH:13][CH:14]=[CH:15]4)=[CH:19][CH:20]=[CH:21][CH:22]=3)=[CH:6][CH:5]=1

参加物

5

反応物 2

HCID 24479Stannous ChlorideHCID 730989559-(4-Nitrostyryl)acridine2 回

生成物 1

HCID 146733HCID 146733、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

The 9-(4-nitrostyryl)acridine product (2.86 g, 10.0 mmol) is dissolved in ethyl acetate (250 ml) and then brought to reflux. A solution of tin(II) chloride dehydrate (9.0 g, 40 mmol) in hot ethanol (150 ml) is cooled and added to the solution of 9-(4-nitrostyryl)acridine. The mixture is reacted under reflux and with stirring for 5 hours. After cooling, the 9-(4-aminostyryl)acridine precipitates and is isolated by filtration under vacuum. The filtrate is dried by evaporation and taken up in water (500 ml) with stirring. The solution is basified (pH 13–14) with a sodium hydroxide solution. The 9-(4-aminostyryl)acridine fraction previously isolated, which contains a high proportion of tin salt, is also basified. The 9-(4-aminostyryl)acridine is separated by filtration, washed with water and dried. It is sufficiently pure for the following step.

後処理

  1. temperatureto reflux
  2. customThe mixture is reacted
  3. temperatureunder reflux
  4. temperatureAfter cooling
  5. customthe 9-(4-aminostyryl)acridine precipitates
  6. customis isolated by filtration under vacuum
  7. customThe filtrate is dried by evaporation
  8. stirringwith stirring

出典と根拠

ORDレコード
ord-5699240b52254bce8e67decfb3b46acb
出典データセット
uspto-grants-2007_05
特許番号
US07223865B2

反応ノート

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