Potassium Carbonate → 2,6-Dichloro-4-methoxypyridine

HRID 594090ノート

反応式

HRID 594090 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N+]([O-])=O)[CH:5]=[C:4]([Cl:11])[N:3]=1.[C:12](=O)([O-])[O-:13].[K+].[K+]>CO>[Cl:1][C:2]1[CH:7]=[C:6]([O:13][CH3:12])[CH:5]=[C:4]([Cl:11])[N:3]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 38410702,6-Dichloro-4-nitropyridine

生成物 1

HCID 33199932,6-Dichloro-4-methoxypyridine収率 88%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
70 °C

実験手順

A mixture of 2,6-dichloro-4-nitropyridine (1.0 equiv.), potassium carbonate (3 equiv.) and methanol (20 equiv.) were heated to 70° C. for 25 min in the microwave. The reaction mixture was diluted with methanol and was decanted from remaining solids. After concentration, the mixture was partitioned between water and EtOAc. The organic phase was washed with brine and dried over sodium sulfate. The solution was concentrated and dried under vacuo to give 2,6-dichloro-4-methoxypyridine in 88% yield. LCMS (m/z) (M+H)=177.9/179.9, Rt=0.72 min.

後処理

  1. customwas decanted
  2. concentrationAfter concentration
  3. customthe mixture was partitioned between water and EtOAc
  4. washThe organic phase was washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationThe solution was concentrated
  7. customdried under vacuo

出典と根拠

ORDレコード
ord-6c7a5f9a523a4876b4d4c9633ffa9243
出典データセット
uspto-grants-2016_01
特許番号
US09242969B2

反応ノート

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