HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylenediamine → HCID 15564119, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | HCID 15564114 | HCID 15564114 | — |
| Reactant | HCID 178418546 | HCID 178418546 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15564119 | HCID 15564119 | — |
Reaction Steps
1.5 G. of 5-n-pentyl-2-(4'-bromo-4-biphenylyl)-pyrimidine are heated at reflux for 22 hours with 2.5 g. of copper-(I) cyanide (content 70%) in 50 ml. of dimethylformamide. After cooling, 25 ml. of 10% aqueous ethylenediamine solution are added and, after stirring for a short time, the mixture is extracted with methylene chloride. The organic extract is shaken with a further 25 ml. of ethylenediamine solution and then washed until neutral. The crude concentrate is chromatographed on silica gel with toluene/1% acetone. Recrystallization of the pure fractions from ethyl acetate yields 5-n-pentyl-2-(4'-cyano-4-biphenylyl)-pyrimidine, having a melting point of 123.5°-124° C. and clearing point of 204.5°-205° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04309539 |
| Source dataset | uspto-grants-1982_01 |
| ORD ID | ord-571cbe0dadca4bf9a1061156b82d97d7 |
| Source note | uspto-grants-1982_01 |