Water → 3-(4-Fluoropiperidin-1-yl)-2-nitropyridine

HRID 451516

反応式

HRID 451516 の反応式
Cl.[F:2][CH:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.C(N(CC)CC)C.FC(F)(F)S(O[C:22]1[C:23]([N+:28]([O-:30])=[O:29])=[N:24][CH:25]=[CH:26][CH:27]=1)(=O)=O.O>CC(N(C)C)=O>[F:2][CH:3]1[CH2:8][CH2:7][N:6]([C:22]2[C:23]([N+:28]([O-:30])=[O:29])=[N:24][CH:25]=[CH:26][CH:27]=2)[CH2:5][CH2:4]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 27591584-Fluoropiperidine hydrochlorideHCID 108802252-Nitropyridin-3-yl trifluoromethanesulfonate

生成物 1

HCID 673355063-(4-Fluoropiperidin-1-yl)-2-nitropyridine

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

反応条件

温度
110 °C

実験手順

To a solution of 4-fluoropiperidine hydrochloride (1.54 g, 11 mmol) and triethylamine (4.5 mL, 33 mmol) in dimethylacetamide (30 mL) was added 2-nitropyridin-3-yl trifluoro-methanesulfonate (3.00 g, 11 mmol) and the mixture heated to 110° C. for 1 hour. Water was added and the mixture extracted with ethyl acetate. The organic phase was washed with brine and dried with sodium sulfate. The solvent was evaporated in vacuo and the product used without further purification. The title compound was obtained as a yellow oil (2.22 g, 89%).

後処理

  1. extractionthe mixture extracted with ethyl acetate
  2. washThe organic phase was washed with brine
  3. dry with materialdried with sodium sulfate
  4. customThe solvent was evaporated in vacuo
  5. customthe product used without further purification

出典と根拠

ORDレコード
ord-b1fc0a0987334b61ba2a9df044f6e036
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

関連ノート

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