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

HRID 2085119
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반응식

HRID 2085119 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
참가 물질실험 절차후처리출처 및 근거반응 노트

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-1823cb7f944843719cac37a7d798050b
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06720320B2

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