Acetic Acid → HCID 70510514、化合物

HRID 1632860ノート

反応式

HRID 1632860 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]2[N:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[N+:24]([O-:26])=[O:25])[CH2:9][C:10]3([CH2:15][CH2:14][N:13](C#N)[CH2:12][CH2:11]3)[C:5]2=[CH:4][CH:3]=1.C(O)(=O)C.[OH-].[Na+].[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([OH:38])=[O:37]>Cl.CCOCC>[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([OH:38])=[O:37].[Cl:1][C:2]1[CH:7]=[C:6]2[N:8]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[N+:24]([O-:26])=[O:25])[CH2:9][C:10]3([CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[C:5]2=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 444266Maleic AcidHCID 128016286-Chloro-1'-cyano-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine]

生成物 1

HCID 70510514HCID 70510514、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 3283Diethyl Ether溶媒

実験手順

A suspension of 2.5 g of 6-chloro-1'-cyano-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine], Example 31, in 40 ml of 3N hydrochloric acid and 20 ml of glacial acetic acid is refluxed for 16 hours under nitrogen. Thereafter, the mixture is permitted to cool before sequentially being basified with dilute sodium hydroxide and extracted with ether. The combined ether extracts are successively washed with water, dried and concentrated under vacuum leaving an oil residue. The residue, in ether, is converted to its maleic acid salt which is recrystallized from an acetone-ether mixture to provide orange prisms, mp 153°-155° C. of 6-chloro-1-(2-nitrophenyl)spiro[indoline-3,4'-piperidine] maleate.

後処理

  1. temperatureto cool
  2. extractionextracted with ether
  3. washThe combined ether extracts are successively washed with water
  4. customdried
  5. concentrationconcentrated under vacuum
  6. customleaving an oil residue
  7. customis recrystallized from an acetone-ether mixture

出典と根拠

ORDレコード
ord-ac364d8eb7c34958af53a6e4958ead4d
出典データセット
uspto-grants-1984_10
特許番号
US04477667

反応ノート

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