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

HRID 561831

反応式

HRID 561831 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
105 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-70df9b98d1eb4805a17df1e360bec669
出典データセット
uspto-grants-2011_11
特許番号
US08063105B2

関連ノート

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