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Piperidine → 5-Phenyl-3-(2-(1-piperidyl)ethoxy)isoxazole

HRID 612928
ノート
印刷プレビュー

反応式

HRID 612928 の反応式
Br[CH2:2][CH2:3][O:4][C:5]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[O:7][N:6]=1.[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>CO>[C:10]1([C:8]2[O:7][N:6]=[C:5]([O:4][CH2:3][CH2:2][N:16]3[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]3)[CH:9]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1
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 8082PiperidineHCID 195964873-(2-Bromoethoxy)-5-phenylisoxazole

生成物 1

HCID 195965575-Phenyl-3-(2-(1-piperidyl)ethoxy)isoxazole収率 92.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

3-(2-Bromoethoxy)-5-phenylisoxazole (268 mg) was dissolved in methanol (1.0 ml), and piperidine (426 mg) was added thereto, followed by reflux of the resulting mixture for 3 hours. After the reaction mixture was added to ice-cold water (20 ml) and extracted with ether (20 ml×2), the organic layer was dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate) to obtain the title compound (251 mg, 92%) as colorless crystals.

後処理

  1. temperatureby reflux of the resulting mixture for 3 hours
  2. extractionextracted with ether (20 ml×2)
  3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationAfter filtration
  5. customthe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate)

出典と根拠

ORDレコード
ord-35a1b20fc1d74e029752a7d3c2b0ec6f
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06005116

反応ノート

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