Hydrochloric Acid → N-(o-(2,2,2-Trifluoroethoxy)phenyl)-4-piperidone

HRID 842795노트

반응식

HRID 842795 반응식
C1O[C:5]2([CH2:10][CH2:9][N:8]([C:11]3[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=3[O:17][CH2:18][C:19]([F:22])([F:21])[F:20])[CH2:7][CH2:6]2)[O:4]C1C.Cl>C(O)(=O)C.O>[F:22][C:19]([F:20])([F:21])[CH2:18][O:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[N:8]1[CH2:7][CH2:6][C:5](=[O:4])[CH2:10][CH2:9]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 57019377N-(2-(2,2,2-Trifluoroethoxy)phenyl)-4-piperidone propylene ketal

생성물 1

HCID 22615386N-(o-(2,2,2-Trifluoroethoxy)phenyl)-4-piperidone

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

A solution of 51 (410 mg, 1.23 mmol) in acetic acid (20 mL), water (20 ml), and concetrated HCl (5 mL) was heated in an oil bath (60° C.) overnight. The solvent was removed in vacuo and the residue dissolved in dichloromethane and sodium bicarbonate solution. The aqueous layer was extracted with two additional portions of dichloromethane and the combined organic extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. PCTLC (SiO2, 4 mm, 10% EtOH-90% CHCl3) afforded the title compound (52)

후처리

  1. customThe solvent was removed in vacuo
  2. dissolutionthe residue dissolved in dichloromethane
  3. extractionThe aqueous layer was extracted with two additional portions of dichloromethane
  4. washthe combined organic extracts were washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-273c4be4a94a4f7cb10e8449a1f55de3
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06376503B1

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