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Water → 7-Chloro-6-(4-fluorophenyl)-imidazo[1,2-a]pyrimidine

HRID 1851150
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HRID 1851150 반응식
Cl[C:2]1[N:7]2[CH:8]=[CH:9][N:10]=[C:6]2[N:5]=[C:4]([Cl:11])[C:3]=1[C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1.C1COCC1.O.[NH4+].[Cl-]>C(O)C.[Zn]>[Cl:11][C:4]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)=[CH:2][N:7]2[CH:8]=[CH:9][N:10]=[C:6]2[N:5]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 862136515,7-Dichloro-6-(4-fluorophenyl)-imidazo[1,2-a]pyrimidine

생성물 1

HCID 867030197-Chloro-6-(4-fluorophenyl)-imidazo[1,2-a]pyrimidine

시약·촉매·용매 2

HCID 23994Zinc촉매
HCID 702
Ethanol
용매

실험 절차

5.3 g (18.9 mmol) 5,7-Dichloro-6-(4-fluorophenyl)-imidazo[1,2-a]pyrimidine are given in 480 mL ethanol, 184 mL THF and 342 mL water. After addition of 4.7 g (89.5 mmol) NH4Cl and 7.9 g (120 mmol) zinc the mixture is vigorously stirred at rt for two and a half hours. The reaction mixture is filtered via a glass microfibre filter and washed with plenty of methanol. The solvent has been removed and the residue redissolved in ethyl acetate (1 L). After washing twice with brine the solvent is evaporated (without prior drying due to solid material in the solvent). 3.83 g (81.8%) of the desired product containing 11% of the bisdeschloro compound are obtained which is used without further purification.

후처리

  1. filtrationThe reaction mixture is filtered via a glass microfibre
  2. filtrationfilter
  3. washwashed with plenty of methanol
  4. customThe solvent has been removed
  5. dissolutionthe residue redissolved in ethyl acetate (1 L)
  6. washAfter washing twice with brine the solvent
  7. customis evaporated (
  8. customwithout prior drying due to solid material in the solvent)
  9. addition3.83 g (81.8%) of the desired product containing 11% of the bisdeschloro compound
  10. customare obtained which
  11. customis used without further purification

출처 및 근거

ORD 기록
ord-1ab23ea887d44b20a1347cd6aeb83fb6
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08957064B2

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