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

HRID 546747노트

반응식

HRID 546747 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-8e8aa8debf314bb6b196e8c90c7bd71b
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935815B2

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