Hydrogen iodide → HCID 86106951, compound

HRID 1977194Notes

Reaction equation

HRID 1977194 reaction equation
[P](I)I.Cl[C:5]1[N:6]=[C:7]([NH:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:8]2[N:13]=[C:12](Cl)[N:11]=[C:10]([NH:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:9]=2[N:22]=1.I>>[NH:23]([C:7]1[C:8]2[N:13]=[CH:12][N:11]=[C:10]([NH:15][C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[C:9]=2[N:22]=[CH:5][N:6]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

Participants

4

Reactant 3

HCID 24841Hydrogen iodideHCID 13828801HCID 13828801, compoundHCID 579804802,6-Dichloro-N~4~,N~8~-diphenylpyrimido[5,4-d]pyrimidine-4,8-diamine

Product 1

HCID 86106951HCID 86106951, compound

Procedure

12 gm. of phosphorus diiodide (P2I4) were added in small portions to a suspension, heated on a steam bath, of 3.8 gm. (0.01) 2,6-dichloro-4,8-dianilino pyrimido-pyrimidine in 40 cc. hydrogen iodide (d=1.7) in the course of about half an hour. Heating was continued for one hour. The mixture was then cooled and the precipitated crystals were filtered off on a vacuum filter. The precipitate was extracted with 200 cc. of hot dioxane. 2.8 gm. of red, brilliant rhombic crystals remained after extraction. The yield was about 90% of the theoretical yield. The crystals were twice recrystallized from dimethyl formamide, whereby very slightly yellowish, small needles having a melting point of 255-256° C. were obtained.

Workup

  1. temperatureheated on a steam bath, of 3.8 gm
  2. customin the course of about half an hour
  3. temperatureHeating
  4. temperatureThe mixture was then cooled
  5. filtrationthe precipitated crystals were filtered off on a vacuum
  6. filtrationfilter
  7. extractionThe precipitate was extracted with 200 cc
  8. extractionafter extraction
  9. customThe crystals were twice recrystallized from dimethyl formamide, whereby very slightly yellowish
  10. customwere obtained

Sources & evidence

ORD record
ord-8252ca0cda394435bdbb0d1007b85c72
Source dataset
uspto-grants-2001_05
Patent number
US06232312B1

Reaction notes

Loading…