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Methane → Anagrelide Hydrochloride Hydrate

HRID 614905
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HRID 614905 반응식
[Cl:1][C:2]1[C:11]([Cl:12])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][N:5]1[CH2:15][C:14](=[O:16])[NH:13][C:6]1=[N:7]2.Cl.C>CO>[OH2:16].[ClH:1].[Cl:1][C:2]1[C:11]([Cl:12])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][N:5]1[CH2:15][C:14](=[O:16])[NH:13][C:6]1=[N:7]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 297MethaneHCID 313Hydrochloric AcidHCID 135409400Anagrelide

생성물 1

HCID 135565321Anagrelide Hydrochloride Hydrate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

6,7-Dichloro-1,5-dihydroimidazo[2,1-b]-quinazolin-2(3H)-one (94.0 g, 0.367 mol) was added to 2.82 liters of boiling methanol. To the suspension was added 77 ml. (0.92 mol) of concentrated hydrochloric acid. A nearly complete solution resulted. Darco G-60 was added, the mixture was boiled for ca. 3 minutes and then filtered. The filtrate was reheated to boiling to effect solution, then cooled slightly, and 1.9 liters of ether added cautiously. The mixture was stirred at ambient temperature for 2 hours and the solid was filtered off. (Crop A).

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후처리

  1. additionTo the suspension was added 77 ml
  2. customA nearly complete solution resulted
  3. filtrationfiltered
  4. temperaturecooled slightly
  5. addition1.9 liters of ether added cautiously
  6. filtrationthe solid was filtered off

출처 및 근거

ORD 기록
ord-ac90729eb582404598dc3d7e155e4a83
출처 데이터셋
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04146718

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