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Hydrochloric Acid → Ethyl 4-tridecylpyrrole-2-carboxylate

HRID 1090751
ノート
印刷プレビュー

反応式

HRID 1090751 の反応式
[H-].[Na+].[CH2:3]([C:16]1[CH:17]=[C:18]([C:21]([OH:23])=[O:22])[NH:19][CH:20]=1)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].Cl.[CH3:25][CH2:26]CCCC>CN(C)C=O>[CH2:3]([C:16]1[CH:17]=[C:18]([C:21]([O:23][CH2:25][CH3:26])=[O:22])[NH:19][CH:20]=1)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8058HexaneHCID 24758Sodium hydrideHCID 99480484-Tridecylpyrrole-2-carboxylic acid

生成物 1

HCID 15023275Ethyl 4-tridecylpyrrole-2-carboxylate収率 55%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

After washing 140 mg (3.50 mmol) of 60% sodium hydride with hexane, 20 ml of dimethylformamide was added thereto, and then 90 mg (3.38 mmol) of 4-tridecylpyrrole-2-carboxylic acid prepared in Example 2 was further added portionwise under stirring at room temperature. After stirring for 10 minutes, 5.0 g (31.8 mmol) of ethyl idodide was added to the reaction solution followed by heating it at 55° C. for 22 hours. After cooling, an aqueous solution of hydrochloric acid was added to acidify the mixture, and the resulting mixture was then extracted with ethyl acetate, washed with an aquous saturated solution of sodium chloride and dried over anhydrous magnesium sulfate. After removing the solvent under reduced pressure, the residue was purified by subjecting it to column chromatography over silica gel (eluent: ethyl acetate/hexane=1/10) to obtain 600 mg (55% yield) of ethyl 4-tridecylpyrrole-2-carboxylate as white crystals, m.p. 59°-60° C.

後処理

  1. additionwas added
  2. stirringAfter stirring for 10 minutes
  3. addition5.0 g (31.8 mmol) of ethyl idodide was added to the reaction solution
  4. temperatureby heating it at 55° C. for 22 hours
  5. temperatureAfter cooling
  6. extractionthe resulting mixture was then extracted with ethyl acetate
  7. washwashed with an aquous saturated solution of sodium chloride
  8. dry with materialdried over anhydrous magnesium sulfate
  9. customAfter removing the solvent under reduced pressure
  10. customthe residue was purified

出典と根拠

ORDレコード
ord-d4b2705470734d879120fc241b20461d
出典データセット
uspto-grants-1992_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05082856

反応ノート

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