Dimethylamine → N-(2-Methoxyphenyl)-4-dimethylaminomethylbenzamide

HRID 2454

反応式

HRID 2454 の反応式
Cl[CH2:2][C:3]1[CH:19]=[CH:18][C:6]([C:7]([NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[O:16][CH3:17])=[O:8])=[CH:5][CH:4]=1.[CH3:20][NH:21][CH3:22]>O1CCOCC1>[CH3:17][O:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[NH:9][C:7](=[O:8])[C:6]1[CH:18]=[CH:19][C:3]([CH2:2][N:21]([CH3:22])[CH3:20])=[CH:4][CH:5]=1

参加物

4

反応物 2

HCID 674DimethylamineHCID 196899684-Chloromethyl-N-(2-methoxyphenyl)benzamide

生成物 1

HCID 19690030N-(2-Methoxyphenyl)-4-dimethylaminomethylbenzamide収率 100%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

In an atmosphere of argon, 4-chloromethyl-N-(2-methoxyphenyl)benzamide (276 mg, 1.0 mmol) was put into a 25 ml capacity eggplant type flask equipped with a cold finger and dissolved in dioxane (3 ml), followed by the addition of 50% dimethylamine aqueous solution (3 ml) at room temperature. After 2.5 hours of stirring at 80° C. and subsequent removal of dioxane by evaporation, the resulting residue was diluted with ethyl acetate (30 ml). The thus diluted solution was dried on anhydrous sodium carbonate, and the resulting residue was purified by subjecting it to a silica gel column chromatography (ether-ethyl acetate-ethyl acetate:methanol=10:1) to obtain 284 mg (100%) of the title compound in the form of colorless oil.

後処理

  1. customequipped with a cold finger
  2. customsubsequent removal of dioxane
  3. customby evaporation
  4. additionthe resulting residue was diluted with ethyl acetate (30 ml)
  5. dry with materialThe thus diluted solution was dried on anhydrous sodium carbonate
  6. customthe resulting residue was purified

出典と根拠

ORDレコード
ord-e6f09e6358c645c8a45e3f4af446ce3d
出典データセット
uspto-grants-1998_03
特許番号
US05728835

関連ノート

読み込み中…