Sodium Methoxide → HCID 12862265、化合物

HRID 1355723ノート

反応式

HRID 1355723 の反応式
[NH2:1][C:2]1[N:7]=[C:6](Cl)[C:5]([C:9]#[N:10])=[C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:3]=1.[CH3:17][O-:18].[Na+]>CO>[NH2:1][C:2]1[N:7]=[C:6]([O:18][CH3:17])[C:5]([C:9]#[N:10])=[C:4]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:3]=1

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 18507370HCID 18507370、化合物

生成物 1

HCID 12862265HCID 12862265、化合物収率 66%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of 200 mg (0.87 mmol) 2-amino-4-chloro-6-phenyl-pyrimidine-5-carbonitrile in 5 ml methanol was added 0.4 ml (2.16 mmol) sodium methylate solution (5.4 M in methanol) and the mixture heated at reflux for 16 h. The reaction mixture was then concentrated in vacuo and the residue partitioned between ethyl acetate and water. The organic phase was dried over sodium sulfate and concentrated in vacuo to afford 130 mg (66%) 2-amino-4-methoxy-6-phenyl-pyrimidine-5-carbonitrile as a light yellow crystalline solid. ES-MS m/e (%): 227 (M+H+, 100).

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 16 h
  3. concentrationThe reaction mixture was then concentrated in vacuo
  4. customthe residue partitioned between ethyl acetate and water
  5. dry with materialThe organic phase was dried over sodium sulfate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-43056bc1817345d0a8b9346db0f1355b
出典データセット
uspto-grants-2003_07
特許番号
US06586441B2

反応ノート

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