4-Chloroaniline → 3-[(4-Chlorophenyl)amino]propan-1-ol

HRID 546747ノート

反応式

HRID 546747 の反応式
[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.F[B-](F)(F)F.[Li+].[O:15]1[CH2:18][CH2:17][CH2:16]1.C(=O)(O)[O-].[Na+]>C(#N)C>[Cl:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][CH2:18][CH2:17][CH2:16][OH:15])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 78124-ChloroanilineHCID 10423OxetaneHCID 516892Sodium BicarbonateHCID 4298216Lithium tetrafluoroborate

生成物 1

HCID 204888633-[(4-Chlorophenyl)amino]propan-1-ol収率 67.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

4-Chloroaniline (4.39 g) and lithium tetrafluoroborate (3.32 g) were added to a solution of oxetane (1.00 g) in acetonitrile (20 mL) at room temperature, and the reaction solution was stirred at room temperature for 52 hours. A saturated sodium bicarbonate solution was added to the reaction solution, followed by extraction with chloroform. The resulting extract was dried over magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system) to obtain 2.17 g of the title compound. The property values of the compound are as follows.

後処理

  1. extractionfollowed by extraction with chloroform
  2. extractionThe resulting extract
  3. dry with materialwas dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)

出典と根拠

ORDレコード
ord-8e8aa8debf314bb6b196e8c90c7bd71b
出典データセット
uspto-grants-2011_05
特許番号
US07935815B2

反応ノート

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