Formic Acid → HCID 22490733, 화합물

HRID 2180863노트

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HRID 2180863 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:16]2[CH:21]=[CH:20][C:19]([NH2:22])=[CH:18][CH:17]=2)[C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][CH:10]=2)=[CH:4][CH:3]=1.[CH:23]([OH:25])=O.Cl.C(N=C=NCCCN(C)C)C.[C:38](OCC)(=[O:40])C.[CH3:44][OH:45]>CN(C)C1C=CN=CC=1.ClCCl.O>[CH:38]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][CH:23]=[O:25])=[CH:11][CH:10]=2)[C:16]2[CH:21]=[CH:20][C:19]([NH:22][CH:44]=[O:45])=[CH:18][CH:17]=2)=[CH:4][CH:3]=1)=[O:40]

참가 물질

9

반응물 5

HCID 284Formic AcidHCID 887MethanolHCID 8857Ethyl AcetateHCID 68356Benzeneamine, 4,4',4''-methylidynetris-HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

생성물 1

HCID 22490733HCID 22490733, 화합물수율 44%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

Tris(4-aminophenyl)methane (2.9 g), formic acid (4.6 g) and 4-dimethylaminopyridine (122 mg) were dissolved in dichloromethane (30 ml), after which 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (9.61 g) was added under a nitrogen atmosphere at 5° C., the temperature was raised to room temperature, and the mixture was stirred for 2 days. Ethyl acetate (100 ml) and water (50 ml) were added to the reaction mixture which was then vigorously shaken, and the organic layer was washed with saturated sodium bicarbonate water (20 ml), water (20 ml) and saturated aqueous sodium chloride (20 ml), dried over sodium sulfate, and concentrated to dryness. The residue was purified by silica gel column chromatography (Kieselgel 60, 240-400 mesh) and elution was performed with a mixed solvent of chloroform:methanol=90:10 to obtain 1.63 g of the title compound as a light brown powder (44% yield).

후처리

  1. stirringwas then vigorously shaken
  2. washthe organic layer was washed with saturated sodium bicarbonate water (20 ml), water (20 ml) and saturated aqueous sodium chloride (20 ml)
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated to dryness
  5. customThe residue was purified by silica gel column chromatography (Kieselgel 60, 240-400 mesh) and elution

출처 및 근거

ORD 기록
ord-268da54416a24a9e9772d9cac32a3eae
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06887890B2

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