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Epichlorohydrin → 1-(Oxiran-2-ylmethyl)piperidine

HRID 420842
ノート
印刷プレビュー

反応式

HRID 420842 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:7]([CH:9]1[O:11][CH2:10]1)Cl.CC(C)([O-])C.[K+]>C(O)(C)(C)C.O1CCCC1>[O:11]1[CH2:10][CH:9]1[CH2:7][N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
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 3

HCID 7835EpichlorohydrinHCID 8082PiperidineHCID 23665647Potassium tert-butoxide

生成物 1

HCID 124018881-(Oxiran-2-ylmethyl)piperidine

試薬・触媒・溶媒 2

HCID 6386tert-Butanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Piperidine (3 ml) was dissolved in t-butyl alcohol (1.2 ml), and the solution was added dropwise with (±)-epichlorohydrin (2.45 ml) on an ice bath. The mixture was slowly warmed to room temperature as it was, and stirred for 18 hours. Then, the mixture was added dropwise with a solution of potassium t-butoxide (3.39 g) in tetrahydrofuran (18 ml) under ice cooling so that the internal temperature should not exceed 15° C. After the addition, the reaction mixture was stirred at room temperature for 2 hours. The reaction mixture was concentrated under reduced pressure, the resulting residue was added to distilled water, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, then dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=50:1) to obtain the title compound (1.55 g).

後処理

  1. customexceed 15° C
  2. additionAfter the addition
  3. stirringthe reaction mixture was stirred at room temperature for 2 hours
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. additionthe resulting residue was added
  6. distillationto distilled water
  7. extractionthe mixture was extracted with chloroform
  8. washThe organic layer was washed with saturated brine
  9. dry with materialdried over anhydrous magnesium sulfate
  10. filtrationfiltered
  11. concentrationThe filtrate was concentrated under reduced pressure
  12. customthe resulting residue was purified by silica gel column chromatography (chloroform:methanol=50:1)

出典と根拠

ORDレコード
ord-4fb34474566e496d9be72f20b7ea5835
出典データセット
uspto-grants-2012_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08097708B2

反応ノート

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