2-Morpholinoethylamine → 5-Bromo-2-(2-morpholinoethylamino)benzonitrile

HRID 380005

反応式

HRID 380005 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5](F)=[C:6]([CH:9]=1)[C:7]#[N:8].[NH2:11][CH2:12][CH2:13][N:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1.C(=O)([O-])O.[Na+]>C(#N)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:11][CH2:12][CH2:13][N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)=[C:6]([CH:9]=1)[C:7]#[N:8]

参加物

5

反応物 3

HCID 4082852-MorpholinoethylamineHCID 516892Sodium BicarbonateHCID 27249005-Bromo-2-fluorobenzonitrile

生成物 1

HCID 183676075-Bromo-2-(2-morpholinoethylamino)benzonitrile収率 49.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

5-Bromo-2-fluorobenzonitrile (1.0 g) and 4-(2-aminoethyl)morpholine (0.65 g) were mixed together in acetonitrile (5 ml) at 70° C. for 4 hours, cooled and poured into a solution of aqueous sodium hydrogen carbonate and was extracted into ethyl acetate, dried over anhydrous magnesium sulfate and concentrated. The residue was purified by chromatography on silica gel eluting with 2.5% methanol in dichloromethane containing 1% triethylamine to afford the sub-titled compound as an oil (0.77 g).

後処理

  1. temperaturecooled
  2. extractionwas extracted into ethyl acetate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by chromatography on silica gel eluting with 2.5% methanol in dichloromethane containing 1% triethylamine

出典と根拠

ORDレコード
ord-f6d5697cacfc4db68e33d05faa7f6052
出典データセット
uspto-grants-2001_10
特許番号
US06300352B1

関連ノート

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