Dimethylformamide → 1-[3,5-Dimethoxy-4-(2-morpholin-4-yl-ethoxy)-phenyl)ethanone

HRID 497032

反応式

HRID 497032 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:12](=[O:14])[CH3:13])[CH:6]=[C:7]([O:10][CH3:11])[C:8]=1[OH:9].Cl.Cl[CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[CH3:11][O:10][C:7]1[CH:6]=[C:5]([C:12](=[O:14])[CH3:13])[CH:4]=[C:3]([O:2][CH3:1])[C:8]=1[O:9][CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][O:22][CH2:21][CH2:20]1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 17198AcetosyringoneHCID 77210Morpholine, 4-(2-chloroethyl)-, hydrochloride (1:1)

生成物 1

HCID 223181171-[3,5-Dimethoxy-4-(2-morpholin-4-yl-ethoxy)-phenyl)ethanone収率 69.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

In a vial, 500 mg (2.5 mmol) of 3′,5′-dimethoxy-4′-hydroxyacetophenone was combined with 4-(2-chloroethyl)morpholine hydrochloride (600 mg, 3.2 mmol), and powdered potassium carbonate (1.5 g, excess). Dimethylformamide (2 mL) was added, the vial was sealed, and the rxn was heated to 80° C. overnight. The reaction was diluted with water and extracted with diethyl ether. The organic extract was washed with brine, dried (Na2SO4), and evaporated in vacuo to afford 540 mg (67%) of 14 as a white solid.

後処理

  1. customthe vial was sealed
  2. extractionextracted with diethyl ether
  3. extractionThe organic extract
  4. washwas washed with brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-25d2e860e6bc4b9cb622bc039d6f7343
出典データセット
uspto-grants-2005_09
特許番号
US06949544B2

関連ノート

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