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

HRID 380005

반응식

HRID 380005 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 183676075-Bromo-2-(2-morpholinoethylamino)benzonitrile수율 49.7%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f6d5697cacfc4db68e33d05faa7f6052
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300352B1

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