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

HRID 451516

반응식

HRID 451516 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

반응 조건

온도
110 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-b1fc0a0987334b61ba2a9df044f6e036
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

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