Sodium Hydroxide → 3-(2-Ethylpyridin-3-yloxy)-5-(pyridin-2-ylthio)picolinamide

HRID 1523578노트

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HRID 1523578 반응식
[CH2:1]([C:3]1[C:8]([O:9][C:10]2[C:11]([C:23]#[N:24])=[N:12][CH:13]=[C:14]([S:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)[CH:15]=2)=[CH:7][CH:6]=[CH:5][N:4]=1)[CH3:2].[OH-:25].[Na+]>S(=O)(=O)(O)O>[CH2:1]([C:3]1[C:8]([O:9][C:10]2[C:11]([C:23]([NH2:24])=[O:25])=[N:12][CH:13]=[C:14]([S:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=3)[CH:15]=2)=[CH:7][CH:6]=[CH:5][N:4]=1)[CH3:2]

참가 물질

4

실험 절차

3-(2-Ethylpyridin-3-yloxy)-5-(pyridin-2-ylthio)picolinonitrile (1.4 g, 4.19 mmol) was stirred in concentrated sulfuric acid (10 mL) overnight at ambient temperature. Ice (100 g) was added and the solution was neutralized using 4M NaOH. Ice was added as necessary to maintain the temperature below 20° C. The product was extracted into ethyl acetate, washed with brine, dried over MgSO4, filtered and concentrated to afford 3-(2-ethylpyridin-3-yloxy)-5-(pyridin-2-ylthio)picolinamide (1.5 g, 4.2 mmol).

후처리

  1. additionIce was added as necessary
  2. temperatureto maintain the temperature below 20° C
  3. extractionThe product was extracted into ethyl acetate
  4. washwashed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d413ae4fd8b345f7b4e415be0108a923
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079890B2

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