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Sodium Hydroxide → HCID 14931744, 화합물

HRID 1252057
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HRID 1252057 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24434Potassium NitrateHCID 14931743HCID 14931743, 화합물

생성물 1

HCID 14931744HCID 14931744, 화합물수율 39.6%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d4840c50c2554ef38ed81dfc11686509
출처 데이터셋
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04742057

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