Formic Acid → HCID 22490733、化合物

HRID 2180863ノート

反応式

HRID 2180863 の反応式
[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]

参加物

9

反応物 5

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

生成物 1

HCID 22490733HCID 22490733、化合物収率 44%

試薬・触媒・溶媒 3

HCID 142844-(Dimethylamino)pyridine触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-268da54416a24a9e9772d9cac32a3eae
出典データセット
uspto-grants-2005_05
特許番号
US06887890B2

反応ノート

読み込み中…