Trimethyl orthoformate → 3-Fluoro-1-(2-fluoro-4-nitrophenyl)-4,4-dimethoxypiperidine

HRID 750907노트

반응식

HRID 750907 반응식
[F:1][CH:2]1C(=O)[CH2:6][CH2:5][N:4]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=2[F:18])[CH2:3]1.[CH3:19][O:20][CH:21](OC)[O:22][CH3:23].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>CO>[CH3:19][O:20][C:21]1([O:22][CH3:23])[CH2:6][CH2:5][N:4]([C:9]2[CH:14]=[CH:13][C:12]([N+:15]([O-:17])=[O:16])=[CH:11][C:10]=2[F:18])[CH2:3][CH:2]1[F:1]

참가 물질

5

반응물 3

HCID 9005Trimethyl orthoformateHCID 521998p-Toluenesulfonic acid monohydrateHCID 597540583-Fluoro-1-(2-fluoro-4-nitrophenyl)piperidin-4-one

생성물 1

HCID 597540593-Fluoro-1-(2-fluoro-4-nitrophenyl)-4,4-dimethoxypiperidine수율 78%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
45 °C

실험 절차

The mixture of 4-(3-fluoro-4-oxo-piperidin-1-yl)-3-fluoronitrobenzene (65 mmol), trimethylorthoformate (130 mmol), p-toluene-sulphonic acid monohydrate (67 mmol) in methanol was heated at 45° C. for 24 hours. Solvent was removed and residual mass was taken into ethyl acetate and saturated sodium bicarbonate solution mixture. The organic layer was dried and removal of the solvent afforded title compound as a solid in 78% yield.

후처리

  1. customSolvent was removed
  2. customThe organic layer was dried
  3. customremoval of the solvent

출처 및 근거

ORD 기록
ord-9381e4ea2cc94baca4866eeed68574ed
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405228B2

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