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Hydrogen iodide → 4,8-Dianilino Pyrimido-Pyrimidine

HRID 1977194
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HRID 1977194 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

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

생성물 1

HCID 861069514,8-Dianilino Pyrimido-Pyrimidine

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8252ca0cda394435bdbb0d1007b85c72
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06232312B1

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