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Sulfuric Acid → HCID 9889248, 화합물

HRID 1840966
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HRID 1840966 반응식
[CH2:1]([O:3][CH2:4][CH2:5][N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)=[CH:7]1)[CH3:2].Cl[C:22]1[CH:32]=[CH:31][C:25](C(OCC)=O)=[C:24]([O:33][CH2:34][CH3:35])[CH:23]=1.[C:36](=[O:39])([O-])[O-:37].[K+].[K+].[OH-].[Na+].S(=O)(=O)(O)O>CCCC(=O)C.C(O)C.O>[CH2:1]([O:3][CH2:4][CH2:5][N:6]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[C:8]([CH:15]2[CH2:16][CH2:17][N:18]([CH2:35][CH2:34][O:33][C:24]3[CH:25]=[CH:31][C:32]([C:36]([OH:37])=[O:39])=[CH:22][CH:23]=3)[CH2:19][CH2:20]2)=[CH:7]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 1118Sulfuric AcidHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 99036001-(2-ethoxyethyl)-3-piperidin-4-yl-1H-indoleHCID 22494013HCID 22494013, 화합물

생성물 1

HCID 9889248HCID 9889248, 화합물수율 65%

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 962Water용매
HCID 78952-Pentanone용매

실험 절차

0.5 g (1.84 mmol) of 4-[1-(2-ethoxy-ethyl)-indol-3-yl]-piperidine and 0.55 g (2.4 mmol) of ethyl 4-chloro-ethoxy-benzoate were disolved in 6 mL of 4-methyl-2-butanone and 0.38 g (2.76 mmol) of potassium carbonate were added. The mixture was refluxed for 18 hours and after cooling, water was added, the organic layer separated, washed with water and brine. The solvent was distilled off. The obtained crude was disolved in 3 mL of ethyl alcohol 96% and 2 mL of a 2N aqueous sodium hydroxide solution were added. After stirring at room temperature for 18 hours the mixture was neutralised with a sulphuric acid solution 10%. The formed solid (0.390 g, 65% yield) was collected, washed with water and dried.

후처리

  1. temperatureThe mixture was refluxed for 18 hours
  2. temperatureafter cooling
  3. customthe organic layer separated
  4. washwashed with water and brine
  5. distillationThe solvent was distilled off
  6. customThe obtained crude

출처 및 근거

ORD 기록
ord-3b063024194341de8f4f501a0b79c4a3
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06683096B2

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