1,4-Dioxane → Methyl 6-chloronicotinimidate

HRID 1020958ノート

反応式

HRID 1020958 の反応式
C[O-].[Na+].[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]#[N:12])=[CH:7][N:6]=1.[O:13]1CCOC[CH2:14]1>CO.CCOC(C)=O.O>[Cl:4][C:5]1[CH:10]=[CH:9][C:8]([C:11](=[NH:12])[O:13][CH3:14])=[CH:7][N:6]=1

参加物

7

反応物 3

HCID 312751,4-DioxaneHCID 51520946-Chloro-3-pyridinecarbonitrileHCID 10942334Sodium Methoxide

生成物 1

HCID 86762380Methyl 6-chloronicotinimidate

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Sodium methoxide (725 mg, 13.42 mmol) was added to a solution of 2-Chloro pyridine-5-carbonitrile (1.8 g, 13.04 mmol) in MeOH:dioxane (40 ml, 1:1) at 0° C., then stirred for 30 minutes at 0° C., and 1 hour at room temperature. The reaction was diluted with EtOAc (200 ml) and H2O (100 ml), organic layer separated, dried over Na2SO4, filtered and solvent evaporated to yield title compound 1BX as a white solid (2.6 g, 100%) MS (MH 171)

後処理

  1. custom1 hour
  2. customat room temperature
  3. customseparated
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customsolvent evaporated

出典と根拠

ORDレコード
ord-3615d29780be4a3081082198416b1932
出典データセット
uspto-grants-2014_05
特許番号
US08716483B2

反応ノート

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