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Piperazine → Piperazine, 1-(1-oxooctadecyl)-

HRID 2248047
ノート
印刷プレビュー

反応式

HRID 2248047 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7](Cl)(=[O:25])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]>O1CCCC1>[C:7]([N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1)(=[O:25])[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4837PiperazineHCID 8212Stearoyl chloride

生成物 1

HCID 10020929Piperazine, 1-(1-oxooctadecyl)-収率 13%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

20 g of anhydrous piperazine was dissolved in 1,000 ml of tetrahydrofuran and then 33.6 g of stearoyl chloride was added dropwise thereto under stirring and under cooling with ice. The mixture was stirred under cooling with ice for 1 h and tetrahydrofuran was distilled off under reduced pressure. A saturated aqueous solution of sodium hydrogencarbonate was added to the residue. After extraction with 200 ml of chloroform three times, the extract was washed with a saturated aqueous solution of common salt and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol=9/1) to obtain 5.1 g of the intended product.

後処理

  1. temperatureunder cooling with ice
  2. stirringThe mixture was stirred
  3. temperatureunder cooling with ice for 1 h
  4. distillationtetrahydrofuran was distilled off under reduced pressure
  5. additionA saturated aqueous solution of sodium hydrogencarbonate was added to the residue
  6. extractionAfter extraction with 200 ml of chloroform three times
  7. washthe extract was washed with a saturated aqueous solution of common salt
  8. distillationthe solvent was distilled off under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol=9/1)

出典と根拠

ORDレコード
ord-947acbcf5e3242249ab0ed0f1ab3f4dd
出典データセット
uspto-grants-1991_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05037827

反応ノート

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