Hydrochloric Acid → Cyclohexanone, 4-(4-pyridinyl)-

HRID 1193342ノート

反応式

HRID 1193342 の反応式
Cl.O1[C:6]2([CH2:11][CH2:10][CH:9]([C:12]3[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=3)[CH2:8][CH2:7]2)[O:5]CC1>C1COCC1>[N:15]1[CH:16]=[CH:17][C:12]([CH:9]2[CH2:8][CH2:7][C:6](=[O:5])[CH2:11][CH2:10]2)=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 578925724-(4-Pyridyl)cyclohexanone ethylene ketal

生成物 1

HCID 10154273Cyclohexanone, 4-(4-pyridinyl)-収率 69%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2 M HCl (13.6 ml) was added to a solution of 4-(1,4-dioxaspiro[4.5]decan-8-yl)pyridine (3.0 g, 13.6 mmol, 1 eq) in THF (136 ml), and stirring was carried out for 3 h at RT. The solvent was removed under reduced pressure. The residue was diluted with water (50 ml) and rendered basic with solid sodium hydrogen carbonate. Then extraction with ethyl acetate (2×100 ml) was carried out. The combined organic phases were washed with water (80 ml), dried over sodium sulfate and concentrated under reduced pressure. The desired product was used in the next step without being purified further. Yield: 69% (1.65 g, 9.42 mmol).

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionThe residue was diluted with water (50 ml)
  3. extractionThen extraction with ethyl acetate (2×100 ml)
  4. washThe combined organic phases were washed with water (80 ml)
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customwithout being purified further

出典と根拠

ORDレコード
ord-173c05bd90a345788de64512bf96573f
出典データセット
uspto-grants-2014_03
特許番号
US08680159B2

反応ノート

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