Ammonia → Fenpiclonil

HRID 247103

反応式

HRID 247103 の反応式
F[C:2](F)(F)[C:3]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[C:9]=2[Cl:15])=[CH:6][NH:5][CH:4]=1.[NH3:18]>O1CCOCC1>[Cl:15][C:9]1[C:10]([Cl:14])=[CH:11][CH:12]=[CH:13][C:8]=1[C:7]1[C:3]([C:2]#[N:18])=[CH:4][NH:5][CH:6]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 212455323-Trifluoromethyl-4-(2,3-dichlorophenyl)-pyrrole

生成物 1

HCID 91724Fenpiclonil

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

4.0 g of 3-trifluoromethyl-4-(2,3-dichlorophenyl)-pyrrole, 21 ml of 25% aqueous ammonia and 40 ml of dioxane are stirred for 26 hours at 180° C. in an autoclave. After cooling to room temperature, the reaction mixture is filtered, and the clear filtrate is concentrated by evaporation. The residue is taken up in ethyl acetate, washed with water and subsequently with diluted sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated by evaporation. The residue is caused to crystallise by the addition of hexane; it is then filtered off and dried to thus obtain 3.4 g (100% of theory) of 4-(2,3-dichlorophenyl)-3-cyanopyrrole having a melting point of 150° C.

後処理

  1. filtrationthe reaction mixture is filtered
  2. concentrationthe clear filtrate is concentrated by evaporation
  3. washwashed with water and subsequently with diluted sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated by evaporation
  7. customto crystallise by the addition of hexane
  8. filtrationit is then filtered off
  9. dry with materialdried to thus obtain 3.4 g (100% of theory) of 4-(2,3-dichlorophenyl)-3-cyanopyrrole having a melting point of 150° C.

出典と根拠

ORDレコード
ord-35c8aa3adda7435983b40f361ae24f35
出典データセット
uspto-grants-1987_11
特許番号
US04705801

関連ノート

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