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

HRID 460547
ノート
印刷プレビュー

反応式

HRID 460547 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-8139e317c96947d291f59e34795c6afa
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07196199B2

反応ノート

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