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

HRID 750907ノート

反応式

HRID 750907 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
45 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9381e4ea2cc94baca4866eeed68574ed
出典データセット
uspto-grants-2008_07
特許番号
US07405228B2

反応ノート

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