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

HRID 594090

반응식

HRID 594090 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 33199932,6-Dichloro-4-methoxypyridine수율 88%

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6c7a5f9a523a4876b4d4c9633ffa9243
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242969B2

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