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

HRID 1851150
ノート
印刷プレビュー

反応式

HRID 1851150 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][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
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23994Zinc触媒
HCID 702
Ethanol
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1ab23ea887d44b20a1347cd6aeb83fb6
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08957064B2

反応ノート

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