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Sodium Hydroxide → HCID 14931744、化合物

HRID 1252057
ノート
印刷プレビュー

反応式

HRID 1252057 の反応式
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([CH:10]2[C:18]3[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=3)[N:12](C(=O)C)[CH2:11]2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[N+:22]([O-])([O-:24])=[O:23].[K+].[OH-].[Na+]>S(=O)(=O)(O)O>[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([CH:10]2[C:18]3[C:13](=[CH:14][CH:15]=[C:16]([N+:22]([O-:24])=[O:23])[CH:17]=3)[NH:12][CH2:11]2)[CH2:6][CH2:5]1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24434Potassium NitrateHCID 14931743HCID 14931743、化合物

生成物 1

HCID 14931744HCID 14931744、化合物収率 39.6%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

To a solution of 3-(1-acetyl-4-piperidyl)-1acetylindoline (0.3 g) in conc. sulfuric acid (5 ml) was added potassium nitrate (0.12 g) in small portions at a temperature not exceeding 10° C. with stirring. The mixture was stirred at the same temperature for 1 hour and at ambient temperature for 7 hours. The reaction mixture was poured into ice and allowed to stand at ambient temperature for 3 days. The aqueous solution was neutralized with 2N aqueous sodium hydroxide solution and extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. The solvent was distilled off and the residue was subjected to column chromatography on silica gel, followed by elution with a mixture of chloroform and methanol to give 3-(1-acetyl-4-piperidyl)-5-nitroindoline (0.12 g).

後処理

  1. customexceeding 10° C.
  2. stirringThe mixture was stirred at the same temperature for 1 hour and at ambient temperature for 7 hours
  3. additionThe reaction mixture was poured into ice
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent was distilled off
  8. washfollowed by elution with a mixture of chloroform and methanol

出典と根拠

ORDレコード
ord-d4840c50c2554ef38ed81dfc11686509
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04742057

反応ノート

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