Triethylamine → HCID 53996767、化合物

HRID 255955

反応式

HRID 255955 の反応式
[CH3:1][N:2]([CH3:7])[CH:3]=[CH:4][C:5]#[N:6].C(N(CC)CC)C.[Cl:15][C:16]1[CH:24]=[C:23]([Cl:25])[C:22]([F:26])=[CH:21][C:17]=1[C:18](Cl)=[O:19]>O1CCOCC1>[CH3:1][N:2]([CH3:7])[CH:3]=[C:4]([C:18](=[O:19])[C:17]1[CH:21]=[C:22]([F:26])[C:23]([Cl:25])=[CH:24][C:16]=1[Cl:15])[C:5]#[N:6]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 974973-(Dimethylamino)prop-2-enenitrileHCID 27368212,4-Dichloro-5-fluorobenzoyl chloride

生成物 1

HCID 53996767HCID 53996767、化合物収率 77.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

9.6 g of 3-dimethylaminoacrylonitrile and 10.5 g of triethylamine are added dropwise to a solution of 22.75 g of 2,4-dichloro-5-fluorobenzoyl chloride in 100 ml of anhydrous dioxane, while cooling in ice and stirring. The mixture is stirred at room temperature for 1 hour and then heated to boiling under reflux for 4 hours. The solvent is removed by distillation in vacuo, and the residue is taken up in methylene chloride/water. The methylene chloride phase is washed with water, dried with sodium sulphate, and evaporated in vacuo. The crystalline residue is recrystallized from ethanol. 22.2 g of 3-dimethylamino-2-(2,4-dichloro-5-fluorobenzoyl)acrylonitrile of melting point 138°-139° C. are obtained.

後処理

  1. temperaturewhile cooling in ice
  2. stirringThe mixture is stirred at room temperature for 1 hour
  3. temperatureheated
  4. temperatureunder reflux for 4 hours
  5. customThe solvent is removed by distillation in vacuo
  6. washThe methylene chloride phase is washed with water
  7. dry with materialdried with sodium sulphate
  8. customevaporated in vacuo
  9. customThe crystalline residue is recrystallized from ethanol

出典と根拠

ORDレコード
ord-79dc08f483de46299a7c81bb61a53f4d
出典データセット
uspto-grants-1987_10
特許番号
US04699992

関連ノート

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