3-Chloro-4-morpholinoaniline → N-(3-chloro-4-morpholinophenyl)-3-oxobutanamide

HRID 56229노트

반응식

HRID 56229 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[N:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1)[NH2:5].[C:15]([CH:18]=[C:19]=[O:20])(=[O:17])[CH3:16]>CCOC(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:5][C:19](=[O:20])[CH2:18][C:15](=[O:17])[CH3:16])[CH:6]=[CH:7][C:8]=1[N:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1

참가 물질

4

반응물 2

HCID 1086613-Chloro-4-morpholinoanilineHCID 12642904But-1-ene-1,3-dione

생성물 1

HCID 90022603N-(3-chloro-4-morpholinophenyl)-3-oxobutanamide수율 91%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 3-chloro-4-morpholinoaniline (2.05 g, 9.64 mmol) in EtOAc (30 mL) was added acetyl ketene (1.62 g, 19.3 mmol) with stirring and the mixture was stirred at 80° C. overnight. The mixture was cooled to rt and concentrated in vacuo. The residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=3:1) to give the title compound as a pale yellow solid (2.59 g, 91%).

후처리

  1. stirringthe mixture was stirred at 80° C. overnight
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=3:1)

출처 및 근거

ORD 기록
ord-37bf6db4682043d784aacf127e737472
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434695B2

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