Cyclopropanecarboxylic acid → HCID 178526476、化合物

HRID 19744

反応式

HRID 19744 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([NH2:10])=[C:6]([NH2:11])[CH:5]=1)([O-:3])=[O:2].[CH:12]1([C:15](O)=O)[CH2:14][CH2:13]1>>[CH:12]1([C:15]2[NH:10][C:7]3[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][C:6]=3[N:11]=2)[CH2:14][CH2:13]1

参加物

3

反応物 2

HCID 15655Cyclopropanecarboxylic acidHCID 51117914-Nitro-1,2-phenylenediamine

生成物 1

HCID 178526476HCID 178526476、化合物収率 98%

実験手順

By analogy with a described method (WO 96/04270), a solution of 5 g (32.65 mmol) of 4-nitro-1,2-phenylenediamine in 77 ml (0.979 mol) of cyclopropanecarboxylic acid is stirred at reflux for 14 hours. The reaction mixture is then concentrated under reduced pressure and taken up in 150 ml of ethyl acetate and 100 ml of sodium hydrogen carbonate. The organic phase is washed with 100 ml of water and then with 50 ml of saturated sodium chloride solution, dried over magnesium sulfate and then concentrated under reduced pressure. 6.5 g of a brown oil are obtained, and are used without further purification in the following step.

後処理

  1. temperatureat reflux for 14 hours
  2. concentrationThe reaction mixture is then concentrated under reduced pressure
  3. washThe organic phase is washed with 100 ml of water
  4. dry with materialwith 50 ml of saturated sodium chloride solution, dried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-4b30a245a00a456e92a94bd884845186
出典データセット
uspto-grants-2010_06
特許番号
US07745467B2

関連ノート

読み込み中…