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

HRID 497032

반응식

HRID 497032 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-25d2e860e6bc4b9cb622bc039d6f7343
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949544B2

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