Cesium carbonate → 2-Methyl-5-(2-methyl-4-nitrophenoxy)pyridine

HRID 877094

반응식

HRID 877094 반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH3:11].[CH3:12][C:13]1[N:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[CH3:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[O:19][C:16]1[CH:15]=[CH:14][C:13]([CH3:12])=[N:18][CH:17]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 142752-Methyl-5-hydroxypyridineHCID 83315Benzene, 1-chloro-2-methyl-4-nitro-

생성물 1

HCID 179901022-Methyl-5-(2-methyl-4-nitrophenoxy)pyridine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

The mixture of 1-chloro-2-methyl-4-nitrobenzene (17.2 g), 6-methylpyridin-3-ol (12 g) and Cs2CO3 (39 g) in DMF (150 mL) was heated at 110° C. for 4 h. The solid was filtered and water (100 mL) and EtOAc (200 mL) were added. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated. The obtained yellow solid was used for the next step directly.

후처리

  1. filtrationThe solid was filtered
  2. additionwater (100 mL) and EtOAc (200 mL) were added
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-33ca47bf8b6d4e3fa5d1d616b29da37c
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08987284B2

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