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

HRID 1608196
ノート
印刷プレビュー

反応式

HRID 1608196 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-26c5b00e446445b7983ad23a036bf683
出典データセット
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04870074

反応ノート

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