m-Chloroperbenzoic acid → HCID 20555083、化合物

HRID 1105814ノート

反応式

HRID 1105814 の反応式
[CH2:1]([O:4][C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-:15])=[O:14])[C:6]=1[C:7]#[N:8])[CH:2]=[CH2:3].ClC1C=CC=C(C(OO)=[O:24])C=1>C(Cl)(Cl)Cl>[O:24]1[CH2:3][CH:2]1[CH2:1][O:4][C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([N+:13]([O-:15])=[O:14])[C:6]=1[C:7]#[N:8]

参加物

4

反応物 2

HCID 70297m-Chloroperbenzoic acidHCID 20555052HCID 20555052、化合物

生成物 1

HCID 20555083HCID 20555083、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

22.5 g of 2-allyloxy-6-nitro-benzonitrile are introduced into a solution of 26.8 g of m-chloroperbenzoic acid (85% strength) in 1 liter of chloroform and the mixture is warmed to 50° in the course of 3 hours. The reaction mixture is kept at this temperature for 24 hours and then cooled and the solution is washed with 100 ml of 1 M sodium sulphite solution, then with 100 ml of 2 N sodium hydroxide solution and finally with 100 ml of water. After drying over magnesium sulphate and evaporating the solution, a colourless crystalline residue is obtained and this is ground with 20 ml of isopropanol, the mixture is filtered and the material on the filter is dried in vacuo, after which crude 2-(2,3-epoxypropoxy)-6-nitro-benzonitrile with a melting point of 131°-135° is obtained and this is used further in the form of the crude product.

後処理

  1. temperaturethe mixture is warmed to 50° in the course of 3 hours
  2. temperaturecooled
  3. washthe solution is washed with 100 ml of 1 M sodium sulphite solution
  4. dry with materialAfter drying over magnesium sulphate
  5. customevaporating the solution
  6. customa colourless crystalline residue is obtained
  7. filtrationthis is ground with 20 ml of isopropanol, the mixture is filtered
  8. customthe material on the filter is dried in vacuo

出典と根拠

ORDレコード
ord-2ce346f31da74bc2b5eee6d7bcd225c3
出典データセット
uspto-grants-1982_01
特許番号
US04310527

反応ノート

読み込み中…