Water → 2-(Methoxymethyl)aniline

HRID 399780

반응식

HRID 399780 반응식
O.C([O-])([O-])=O.[Na+].[Na+].[OH-].[Na+].[CH3:10][O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[N+:19]([O-])=O>CO.CCOCC>[CH3:10][O:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[NH2:19]

참가 물질

7

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 126166891-(Methoxymethyl)-2-nitrobenzene

생성물 1

HCID 123343062-(Methoxymethyl)aniline수율 101.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 3283Diethyl Ether용매

실험 절차

528 g of 21.8% strength Na2 [Fe(CO)4 ] solution (0.6 mol; 1 kg of the solution contains 633 g of water, 218 g of Na2 [Fe(CO)4 ], 108 g of Na2CO3 and 41 g of NaOH) are added dropwise to 101 g (0.6 mol) of o-methoxymethylnitrobenzene (Example 3a) in 1 l of methanol at 20°-30° C. Stirring is carried out for 1 hour at room temperature, after which the reaction mixture is diluted with ether. A brown oil separates out in the reaction vessel. The total reaction mixture is poured onto a silica gel column and is eluted with ether. Thereafter, the ether phase is evaporated, the residue is taken up in methylene chloride and the solution is dried over MgSO4. It is filtered under suction over silica gel and the solvent is then evaporated off under reduced pressure. The residue is purified by column chromatography with hexane and methylene chloride. 83.8 g of o-methoxymethylaniline are obtained as a brown oil, which is directly reacted further.

후처리

  1. customThe total reaction mixture
  2. additionis poured onto a silica gel column
  3. washis eluted with ether
  4. customThereafter, the ether phase is evaporated
  5. dry with materialthe solution is dried over MgSO4
  6. filtrationIt is filtered under suction over silica gel
  7. customthe solvent is then evaporated off under reduced pressure
  8. customThe residue is purified by column chromatography with hexane and methylene chloride

출처 및 근거

ORD 기록
ord-6c69e0ce99d441449627f86473f8a618
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05824705

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