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

HRID 1820862노트

반응식

HRID 1820862 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매3회

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-cf6c75d5631741feb3083f64c3dddc10
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07605176B2

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