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

HRID 1193342노트

반응식

HRID 1193342 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-173c05bd90a345788de64512bf96573f
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680159B2

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