Diisopropylethylamine → Ethyl 4-[2-(1-ethylpropyl)-1H-imidazol-1-yl]-3-nitrobenzoate

HRID 2068969

반응식

HRID 2068969 반응식
F[C:2]1[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]=1[N+:13]([O-:15])=[O:14].[CH2:16]([CH:18]([C:21]1[NH:22][CH:23]=[CH:24][N:25]=1)[CH2:19][CH3:20])[CH3:17].C(N(CC)C(C)C)(C)C>C(#N)C>[CH2:16]([CH:18]([C:21]1[N:22]([C:2]2[CH:12]=[CH:11][C:5]([C:6]([O:8][CH2:9][CH3:10])=[O:7])=[CH:4][C:3]=2[N+:13]([O-:15])=[O:14])[CH:23]=[CH:24][N:25]=1)[CH2:19][CH3:20])[CH3:17]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 2411062-pentan-3-yl-1H-imidazoleHCID 21277355Ethyl 4-fluoro-3-nitrobenzoate

생성물 1

HCID 59198861Ethyl 4-[2-(1-ethylpropyl)-1H-imidazol-1-yl]-3-nitrobenzoate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Ethyl 4-fluoro-3-nitrobenzoate 9.16 g, 2-(1-ethylpropyl)-1H-imidazole 5.94 g, N,N-diisopropylethylamine 11.2 mL and acetonitrile 86 mL were mixed and heated under reflux for 15 hours in nitrogen atmosphere. From the reaction liquid the solvent was distilled off, and the residue was dissolved in ethyl acetate and rendered weakly alkaline with saturated aqueous sodium hydrogencarbonate solution. The organic layer was separated, washed with water and dried over magnesium sulfate. Distilling the solvent off, 13.16 g of the title compound was obtained.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 15 hours in nitrogen atmosphere
  3. customFrom the reaction liquid the solvent
  4. distillationwas distilled off
  5. dissolutionthe residue was dissolved in ethyl acetate
  6. customThe organic layer was separated
  7. washwashed with water
  8. dry with materialdried over magnesium sulfate
  9. distillationDistilling the solvent off, 13.16 g of the title compound
  10. customwas obtained

출처 및 근거

ORD 기록
ord-f044c0cdabaf448baeef2d7b821eeee2
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299080B2

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