Diethylamine → 2-Chloro-N,N-diethyl-4-nitrobenzeneacetamide

HRID 1820862ノート

反応式

HRID 1820862 の反応式
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[Cl:6][C:7]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[CH:9][C:8]=1[CH2:16][C:17](Cl)=[O:18]>C(OCC)(=O)C>[Cl:6][C:7]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[CH:10]=[CH:9][C:8]=1[CH2:16][C:17]([N:3]([CH2:4][CH3:5])[CH2:1][CH3:2])=[O:18]

参加物

4

反応物 2

HCID 8021DiethylamineHCID 85969188(2-Chloro-4-nitrophenyl)acetic acid chloride

生成物 1

HCID 688195332-Chloro-N,N-diethyl-4-nitrobenzeneacetamide

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒3 回

実験手順

5.67 mL (54.0 mmol) of diethylamine is dissolved in 50 mL of ethyl acetate and 3.20 g (13.7 mmol) of (2-chloro-4-nitrophenyl)acetic acid chloride (VI.1.a) in 50 mL of ethyl acetate is slowly added dropwise at 0° C. Then the mixture is stirred for another 2 hours at ambient temperature. After this time, some more ethyl acetate is added and the mixture is washed twice with water and twice with saturated saline solution. The organic phase is dried over sodium sulfate, the solvent is eliminated and the residue is dried in vacuo. Yield: 3.70 g (100% of theory); Rf value: 0.45 (silica gel, petroleum ether/ethyl acetate=1:1); C12H15ClN2O3; EII mass spectrum: m/z=271/273 [M+H]+.

後処理

  1. washthe mixture is washed twice with water and twice with saturated saline solution
  2. dry with materialThe organic phase is dried over sodium sulfate
  3. customthe residue is dried in vacuo

出典と根拠

ORDレコード
ord-cf6c75d5631741feb3083f64c3dddc10
出典データセット
uspto-grants-2009_10
特許番号
US07605176B2

反応ノート

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