1,2-Dichloroethane → 59855-03-7

HRID 1973585Notes

Reaction equation

HRID 1973585 reaction equation
C([C:5]1[CH:10]=[CH:9][N:8]=[C:7]([C:11]2[CH:19]=[CH:18][C:14]([C:15]([NH2:17])=O)=[CH:13][CH:12]=2)[N:6]=1)CCC.[CH2:20](Cl)[CH2:21]Cl.P(Cl)(Cl)(Cl)=O.[CH3:29][CH2:30]OCC>>[CH2:29]([C:10]1[CH:9]=[N:8][C:7]([C:11]2[CH:12]=[CH:13][C:14]([C:15]#[N:17])=[CH:18][CH:19]=2)=[N:6][CH:5]=1)[CH2:30][CH2:20][CH3:21]

Participants

5

Reactant 4

HCID 111,2-DichloroethaneHCID 3283Diethyl EtherHCID 24813Phosphorus oxychlorideHCID 53928724HCID 53928724, compound

Product 1

HCID 60672259855-03-7

Procedure

11.23 G. of 4-(4-n-butylpyrimid-2-yl)-benzoic acid amide are maintained at reflux for 90 minutes in a mixture of 250 ml. of ethylene chloride and 4.5 ml. of phosphorus oxychloride with stirring. The mixture, diluted with ether, is washed with 2-N sodium hydroxide and then with water until neutral. The organic phase is dried over sodium sulfate and evaporated to give 11.77 g. of 5-n-butyl-2-(4-cyanophenyl)-pyrimidine which are distilled in a high vacuum; melting point 60.9°-61.8° C.

Workup

  1. temperatureat reflux for 90 minutes in a mixture of 250 ml
  2. washis washed with 2-N sodium hydroxide
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customevaporated
  5. customto give 11.77 g
  6. distillationof 5-n-butyl-2-(4-cyanophenyl)-pyrimidine which are distilled in a high vacuum

Sources & evidence

ORD record
ord-8a270186b6314d76bef801366a03bff4
Source dataset
uspto-grants-1976_12
Patent number
US03997536

Reaction notes

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