Hydrogen Bromide → HCID 19790388, 화합물

HRID 2372920노트

반응식

HRID 2372920 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 19790388HCID 19790388, 화합물수율 24%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-db37f8417f2541b684e9f6c6171fc4e5
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05101042

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