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

HRID 842795ノート

反応式

HRID 842795 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

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)

後処理

  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

出典と根拠

ORDレコード
ord-273c4be4a94a4f7cb10e8449a1f55de3
出典データセット
uspto-grants-2002_04
特許番号
US06376503B1

反応ノート

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