5,7-Dichloro-6-(2-fluorophenyl)-imidazo[1,2-a]pyrimidine → 7-Chloro-6-(2-fluorophenyl)-imidazo[1,2-a]pyrimidine

HRID 1851153노트

반응식

HRID 1851153 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][CH:15]=[CH:14][C:13]=1[F:18]>CO.C1COCC1.[Zn].[Cu]>[Cl:11][C:4]1[C:3]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[F:18])=[CH:2][N:7]2[CH:8]=[CH:9][N:10]=[C:6]2[N:5]=1

참가 물질

5

반응물 1

HCID 862136385,7-Dichloro-6-(2-fluorophenyl)-imidazo[1,2-a]pyrimidine

생성물 1

HCID 867030217-Chloro-6-(2-fluorophenyl)-imidazo[1,2-a]pyrimidine

시약·촉매·용매 3

HCID 10290809Zinc copper couple촉매HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

0.86 g (3.05 mmol) 5,7-Dichloro-6-(2-fluorophenyl)-imidazo[1,2-a]pyrimidine are given in 1.5 mL methanol and 8.6 mL THF. After addition of 0.589 g (4.6 mmol) zinc/copper pair the mixture is stirred at rt for 18 hours. The reaction mixture is filtered via a glass microfibre filter and washed with plenty of methanol. The solvent is evaporated and the residue is treated and evaporated three times with toluene. After chromatography on silicagel (eluents dichloromethane/methanol) 672.4 mg (89%) of the desired product containing 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 is evaporated
  5. additionthe residue is treated
  6. customevaporated three times with toluene
  7. additionAfter chromatography on silicagel (eluents dichloromethane/methanol) 672.4 mg (89%) of the desired product containing bisdeschloro compound
  8. customare obtained which
  9. customis used without further purification

출처 및 근거

ORD 기록
ord-b163a4f7327e4663b21343c0487ed35a
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957064B2

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