Dimethylformamide → 3-Bromo-6-methoxy-2,4-dimethylpyridine

HRID 1043889ノート

反応式

HRID 1043889 の反応式
[Br:1][C:2]1[C:3]([CH3:10])=[N:4][C:5](Cl)=[CH:6][C:7]=1[CH3:8].CN([CH:14]=[O:15])C.C[O-].[Na+]>O>[Br:1][C:2]1[C:3]([CH3:10])=[N:4][C:5]([O:15][CH3:14])=[CH:6][C:7]=1[CH3:8]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 10942334Sodium MethoxideHCID 714643513-Bromo-6-chloro-2,4-dimethylpyridine

生成物 1

HCID 112413813-Bromo-6-methoxy-2,4-dimethylpyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

3-bromo-6-chloro-2,4-dimethylpyridine obtained in Preparation Example 21 (200 mg) was added to DMF (1 mL). Sodium methoxide (28% solution in methanol, 0.741 mL) was added to the solution, and the mixture was stirred at 60° C. for 15 hours. Water was added to the reaction mixture, followed by extraction with diethyl ether. The organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 10%) to give the title compound (172 mg).

後処理

  1. extractionfollowed by extraction with diethyl ether
  2. concentrationThe organic layer was concentrated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (ethyl acetate/n-heptane, 0% to 10%)

出典と根拠

ORDレコード
ord-9d9fa4fc783643cb9777faa0cab256b9
出典データセット
uspto-grants-2013_10
特許番号
US08563565B2

反応ノート

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