Methanol → HCID 21094286、化合物

HRID 1350075ノート

反応式

HRID 1350075 の反応式
[CH:1]([NH:3][CH2:4][CH:5]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[CH:11]=1)[C:6]([O:8][CH3:9])=[O:7])=O.P(Cl)(Cl)([Cl:20])=O.CO>C(#N)C>[ClH:20].[CH3:17][O:16][C:12]1[CH:11]=[C:10]2[C:15](=[CH:14][CH:13]=1)[CH:1]=[N:3][CH2:4][CH:5]2[C:6]([O:8][CH3:9])=[O:7]

参加物

5

反応物 3

HCID 887MethanolHCID 24813Phosphorus oxychlorideHCID 21094283HCID 21094283、化合物

生成物 1

HCID 21094286HCID 21094286、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

The compound obtained in Step C (8.03 g; 0.03 mol) is dissolved in 100 ml of acetonitrile, and then the reaction mixture is heated to approximately 60° C. Phosphorus oxychloride (16 ml; 0.17 mol) is added to the solution, which is then heated at reflux for 6 hours with stirring and subsequently evaporated under reduced pressure. The residue obtained is taken up twice with methanol and evaporated under reduced pressure, and then taken up in a minimum of acetone. The precipitate formed is then suction-filtered off to yield the title product in the form of a white solid.

後処理

  1. temperatureis then heated
  2. temperatureat reflux for 6 hours
  3. customsubsequently evaporated under reduced pressure
  4. customThe residue obtained
  5. customevaporated under reduced pressure
  6. customThe precipitate formed
  7. filtrationis then suction-filtered off

出典と根拠

ORDレコード
ord-14379690d01e42d8a8d92c99f150bb9d
出典データセット
uspto-grants-2007_05
特許番号
US07214689B2

反応ノート

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