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Potassium Hydroxide → Benzamide, 4-amino-5-chloro-2-methoxy-N-(2-morpholinylmethyl)-

HRID 1608196
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반응식

HRID 1608196 반응식
[NH2:1][C:2]1[C:22]([Cl:23])=[CH:21][C:5]([C:6]([NH:8][CH2:9][CH:10]2[O:15][CH2:14][CH2:13][N:12](C(OCC)=O)[CH2:11]2)=[O:7])=[C:4]([O:24][CH3:25])[CH:3]=1.[OH-].[K+]>C(O)(C)C>[NH2:1][C:2]1[C:22]([Cl:23])=[CH:21][C:5]([C:6]([NH:8][CH2:9][CH:10]2[O:15][CH2:14][CH2:13][NH:12][CH2:11]2)=[O:7])=[C:4]([O:24][CH3:25])[CH:3]=1
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참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 148773964-amino-5-chloro-N-[(4-ethoxycarbonyl-2-morpholinyl)methyl]-2-methoxybenzamide

생성물 1

HCID 10859540Benzamide, 4-amino-5-chloro-2-methoxy-N-(2-morpholinylmethyl)-수율 28.5%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 4-amino-5-chloro-N-[(4-ethoxycarbonyl-2-morpholinyl)methyl]-2-methoxybenzamide (6.1 g), potassium hydroxide (10.1 g), and isopropyl alcohol (60 ml) is refluxed with stirring for 3 hours. The reaction mixture is concentrated under reduced pressure, and the residue is diluted with water and extracted with chloroform. The organic layer is washed successively with water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The solvent is distilled off under reduced pressure, and the residue is recrystallized from isopropyl alcohol to give the title compound (1.4 g), mp 161°-162° C.

후처리

  1. temperatureis refluxed
  2. concentrationThe reaction mixture is concentrated under reduced pressure
  3. additionthe residue is diluted with water
  4. extractionextracted with chloroform
  5. washThe organic layer is washed successively with water and saturated aqueous sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. distillationThe solvent is distilled off under reduced pressure
  8. customthe residue is recrystallized from isopropyl alcohol

출처 및 근거

ORD 기록
ord-26c5b00e446445b7983ad23a036bf683
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04870074

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