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

HRID 1851153ノート

反応式

HRID 1851153 の反応式
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

参加物

5

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 10290809Zinc copper couple触媒HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b163a4f7327e4663b21343c0487ed35a
出典データセット
uspto-grants-2015_02
特許番号
US08957064B2

反応ノート

読み込み中…