Sodium Methoxide → 2-Chloro-N-cyclopropyl-6-methoxyisonicotinamide

HRID 561831

반응식

HRID 561831 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12](Cl)[N:13]=1)[C:5]([NH:7][CH:8]1[CH2:10][CH2:9]1)=[O:6].[CH3:15][O-:16].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([CH:11]=[C:12]([O:16][CH3:15])[N:13]=1)[C:5]([NH:7][CH:8]1[CH2:10][CH2:9]1)=[O:6]

참가 물질

4

반응물 2

HCID 10942334Sodium MethoxideHCID 215100262,6-Dichloro-N-cyclopropylisonicotinamide

생성물 1

HCID 845809352-Chloro-N-cyclopropyl-6-methoxyisonicotinamide

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
105 °C

실험 절차

To a solution of 2,6-dichloro-N-cyclopropylisonicotinamide from the previous step (1 eq.) in methanol (0.2 M) was added sodium methoxide (6 eq.). The reaction vessel was sealed and the resulting solution was heated in the microwave at 105° C. for 30 min. The volatiles were removed in vacuo and the resulting residue was partitioned between sat. aq. NH4Cl and EtOAc. The organic layer was separated and washed further with brine. Drying over Na2SO4, filtration and concentration of the filtrate in vacuo afforded the title compound as a white solid.

후처리

  1. customThe reaction vessel was sealed
  2. customThe volatiles were removed in vacuo
  3. customthe resulting residue was partitioned between sat. aq. NH4Cl and EtOAc
  4. customThe organic layer was separated
  5. washwashed further with brine
  6. dry with materialDrying over Na2SO4, filtration and concentration of the filtrate in vacuo

출처 및 근거

ORD 기록
ord-70df9b98d1eb4805a17df1e360bec669
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063105B2

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