Water → 2-(4-Diethylamino-but-2-ynyl)-isoindole-1,3-dione

HRID 1620545ノート

反応式

HRID 1620545 の反応式
Cl[CH2:2][C:3]#[C:4][CH2:5][N:6]1[C:14](=[O:15])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]1=[O:16].[CH2:17]([NH:19][CH2:20][CH3:21])[CH3:18].O>C(#N)C>[CH2:17]([N:19]([CH2:20][CH3:21])[CH2:2][C:3]#[C:4][CH2:5][N:6]1[C:14](=[O:15])[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7]1=[O:16])[CH3:18]

参加物

5

反応物 3

HCID 962WaterHCID 8021DiethylamineHCID 2375372-(4-chlorobut-2-yn-1-yl)-2,3-dihydro-1H-isoindole-1,3-dione

生成物 1

HCID 443855092-(4-Diethylamino-but-2-ynyl)-isoindole-1,3-dione収率 48.4%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 2-(4-chlorobut-2-yn-1-yl)-1H-isoindole-1,3(2H)-dione (200 mg) in acetonitrile (3 mL) was added diethylamine (188 mg) at room temperature. The reaction mixture was stirred at room temperature for 4 hr, and added to water at room temperature, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate, and filtered. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (112 mg).

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was evaporated under reduced pressure
  6. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-f875eabe0269457aabbd2ab09d9b45f0
出典データセット
uspto-grants-2014_07
特許番号
US08772277B2

反応ノート

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