Hydrogen Bromide → HCID 19790388、化合物

HRID 1656133ノート

反応式

HRID 1656133 の反応式
[BrH:1].[Cl:2][C:3]1[CH:4]=[C:5]([CH:14]=[CH:15][C:16]=1[Cl:17])[C:6](=O)[CH2:7][CH:8]([C:11]#[N:12])[C:9]#[N:10]>CCOCC.C(Cl)(Cl)Cl>[Br:1][C:9]1[NH:10][C:6]([C:5]2[CH:14]=[CH:15][C:16]([Cl:17])=[C:3]([Cl:2])[CH:4]=2)=[CH:7][C:8]=1[C:11]#[N:12]

参加物

5

反応物 2

HCID 260Hydrogen BromideHCID 10857979Propanedinitrile, [2-(3,4-dichlorophenyl)-2-oxoethyl]-

生成物 1

HCID 19790388HCID 19790388、化合物収率 24%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6212Chloroform溶媒

実験手順

Hydrogen bromide gas is bubbled through a mixture of (3,4-dichlorophenacyl)malononitrile (10.0 g, 0.0395 mol) in ether (150 mL) and chloroform (100 mL) at a moderate rate, keeping the reaction mixture temperature below 35°-40° C. After ten minutes, TLC shows the reaction is complete by UV analysis. The reaction mixture is poured into an ice-water mixture, the layers are separated and the aqueous layer is extracted with ether. The combined organic layer and ether extracts are dried and concentrated in vacuo to give a brown solid. The brown solid is washed with methylene chloride and filtered to obtain the title compound as an off-white solid (3.0 g, 24%, mp >200° C.) which is identified by IR and NMR spectral analyses.

後処理

  1. customthe reaction mixture temperature below 35°-40° C
  2. waitAfter ten minutes
  3. customthe layers are separated
  4. extractionthe aqueous layer is extracted with ether
  5. dry with materialThe combined organic layer and ether extracts are dried
  6. concentrationconcentrated in vacuo
  7. customto give a brown solid
  8. washThe brown solid is washed with methylene chloride
  9. filtrationfiltered

出典と根拠

ORDレコード
ord-05a7a63283b94b4e964b23c899f6f647
出典データセット
uspto-grants-1993_10
特許番号
US05252746

反応ノート

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