Potassium Iodide → N-({4-[(4-Fluorophenyl)methyl]morpholin-2-yl}methyl)acetamide

HRID 1608210ノート

反応式

HRID 1608210 の反応式
[C:1]([NH:4][CH2:5][CH:6]1[O:11][CH2:10][CH2:9][NH:8][CH2:7]1)(=[O:3])[CH3:2].[F:12][C:13]1[CH:20]=[CH:19][C:16]([CH2:17]Cl)=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>C(C(C)=O)C>[C:1]([NH:4][CH2:5][CH:6]1[O:11][CH2:10][CH2:9][N:8]([CH2:17][C:16]2[CH:19]=[CH:20][C:13]([F:12])=[CH:14][CH:15]=2)[CH2:7]1)(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 96024-Fluorobenzyl chlorideHCID 11430Potassium CarbonateHCID 10241064N-(morpholin-2-ylmethyl)acetamide

生成物 1

HCID 10683176N-({4-[(4-Fluorophenyl)methyl]morpholin-2-yl}methyl)acetamide収率 78.9%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 2-acetylaminomethylmorpholine (7.0 g), 4-fluorobenzyl chloride (12 g), potassium carbonate (56 g), potassium iodide (1 g), and methyl ethyl ketone (100 ml) is refluxed with stirring for 17 hours. The reaction mixture is filtered and the filtrate is concentrated under reduced pressure. The residue is diluted with water and extracted with chloroform. The organic layer is separated, 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 toluene to give the title compound (9.3 g), mp 120°-122° C.

後処理

  1. temperatureis refluxed
  2. filtrationThe reaction mixture is filtered
  3. concentrationthe filtrate is concentrated under reduced pressure
  4. additionThe residue is diluted with water
  5. extractionextracted with chloroform
  6. customThe organic layer is separated
  7. washwashed successively with water and saturated aqueous sodium chloride solution
  8. dry with materialdried over magnesium sulfate
  9. distillationThe solvent is distilled off under reduced pressure
  10. customthe residue is recrystallized from toluene

出典と根拠

ORDレコード
ord-1e6ab4cb163145839771db2808f111a3
出典データセット
uspto-grants-1989_09
特許番号
US04870074

反応ノート

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