Water → 5-(N-formyl-N-methylamino-methyl)-2-nitrobenzoic acid methyl ester

HRID 557448노트

반응식

HRID 557448 반응식
[CH:1]([N:3]([CH2:5][C:6]1[CH:7]=[CH:8][C:9]([N+:15]([O-:17])=[O:16])=[C:10]([CH:14]=1)[C:11]([OH:13])=[O:12])[CH3:4])=[O:2].[C:18](=O)([O-])[O-].[K+].[K+].CI.O>CN(C)C=O.C(OCC)(=O)C>[CH3:18][O:12][C:11](=[O:13])[C:10]1[CH:14]=[C:6]([CH2:5][N:3]([CH:1]=[O:2])[CH3:4])[CH:7]=[CH:8][C:9]=1[N+:15]([O-:17])=[O:16]

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 580183265-[[Formyl(methyl)amino]methyl]-2-nitro-benzoic acid

생성물 1

HCID 580183255-(N-formyl-N-methylamino-methyl)-2-nitrobenzoic acid methyl ester수율 124.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

There was dissolved, in 6.8 mL of N,N-dimethylformamide, 3.40 g of 5-(N-formyl-N-methylamino-methyl)-2-nitrobenzoic acid, thereafter 3.94 g of potassium carbonate and 1.77 mL of methyl iodide were added to the solution and then the solution was stirred at a temperature ranging from 20 to 30° C. for 4 hours. After the confirmation of the disappearance of the starting material by HPLC, 20.5 mL of water and 34 mL of ethyl acetate were added to the reaction solution. The organic phase was separated from the aqueous phase, followed by the concentration thereof to give 4.47 g of the intended compound as a crude product (oily state).

후처리

  1. customThe organic phase was separated from the aqueous phase
  2. concentrationfollowed by the concentration

출처 및 근거

ORD 기록
ord-38a8721a0a7a4e2b89272d27121caf9c
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08058432B2

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