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Water → 4-(8-methoxy-2H-chromen-3-ylcarbonyl)morpholine

HRID 460547
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HRID 460547 반응식
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[O:11][CH2:10][C:9]([C:13]([OH:15])=O)=[CH:8]2.[CH2:16]([N:18](CC)[CH2:19][CH3:20])[CH3:17].P(C#N)(OCC)(OCC)=[O:24].O>CN(C=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[O:11][CH2:10][C:9]([C:13]([N:18]1[CH2:19][CH2:20][O:24][CH2:17][CH2:16]1)=[O:15])=[CH:8]2
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참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 76257Diethyl cyanophosphonateHCID 27638908-Methoxy-2H-chromene-3-carboxylic acid

생성물 1

HCID 107548644-(8-methoxy-2H-chromen-3-ylcarbonyl)morpholine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution (200 ml) of 8-methoxy-2H-chromene-3-carboxylic acid (10.0 g) in DMF were added triethylamine (8.6 ml) and diethyl cyanophosphate (10.0 ml) and the mixture was stirred at room temperature for 3 hr. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (chloroform/ethyl acetate) to give the title compound (3.5 g) as a brown oil.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (chloroform/ethyl acetate)

출처 및 근거

ORD 기록
ord-8139e317c96947d291f59e34795c6afa
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07196199B2

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