Heptanoic Acid → Heptanoic acid [2-(4-nitro-phenyl)-ethyl]-amide

HRID 47827

反応式

HRID 47827 の反応式
Cl.CN(C)CCCN=C=NCC.[C:13]([OH:21])(=O)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19].[N+:22]([C:25]1[CH:33]=[CH:32][C:28]([CH2:29][CH2:30][NH2:31])=[CH:27][CH:26]=1)([O-:24])=[O:23].C(N(CC)CC)C>C(OCC)(=O)C.C(Cl)Cl>[N+:22]([C:25]1[CH:26]=[CH:27][C:28]([CH2:29][CH2:30][NH:31][C:13](=[O:21])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])=[CH:32][CH:33]=1)([O-:24])=[O:23]

参加物

7

反応物 4

HCID 8094Heptanoic AcidHCID 8471TriethylamineHCID 951534-NitrophenethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 86586370Heptanoic acid [2-(4-nitro-phenyl)-ethyl]-amide収率 81.3%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (3.86 g, 20.1 mmol) and heptanoic acid (2.38 mL, 16.8 mmol) were added sequentially to a solution of 4-nitrophenethylamine (3.40 g, 16.8 mmol), triethylamine (2.81 mL, 20.1 mmol) and methylene chloride (25 mL). After stirring 18 h at ambient temperature, the reaction mixture was diluted with ethyl acetate; washed sequentially with water, 1N aqueous hydrochloric acid, water, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride; dried over anhydrous sodium sulfate; filtered and concentrated under reduced pressure to provide 3.80 g (81%) of heptanoic acid [2-(4-nitro-phenyl)-ethyl]-amide as an off-white solid.

後処理

  1. washwashed sequentially with water, 1N aqueous hydrochloric acid, water, saturated aqueous sodium bicarbonate and saturated aqueous sodium chloride
  2. dry with materialdried over anhydrous sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a111074eabfd4a1fb8dcd2b34b409831
出典データセット
uspto-grants-2004_03
特許番号
US06699904B2

関連ノート

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