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Sulfuric Acid → HCID 9889248、化合物

HRID 1840966
ノート
印刷プレビュー

反応式

HRID 1840966 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

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

生成物 1

HCID 9889248HCID 9889248、化合物収率 65%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 78952-Pentanone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-3b063024194341de8f4f501a0b79c4a3
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06683096B2

反応ノート

読み込み中…

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