반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1>C(#N)C>[CH2:2]([N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15]참가 물질
4
실험 절차
In a 250-mL round bottom flask, equipped with a magnetic stirrer, a heating mantle and reflux condenser, were placed 1-bromotetradecane (15.9 g, 57.3 mmol), acetonitrile (75 mL), and morpholine (10 g, 114.7 mmol). The reaction mixture was refluxed for 4 hrs. The reaction mixture was cooled to room temperature and was concentrated to a residue on a rotary evaporator. Water and ethyl acetate were added. The organic phase was separated and washed with saturated sodium chloride solution, and then dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated to dryness affording 15.2 g (94% yield) of 4-tetradecylmorpholine as a tan oil. This intermediate was subjected to the next step without further purification.
후처리
- customIn a 250-mL round bottom flask, equipped with a magnetic stirrer
- temperaturea heating mantle and reflux condenser
- temperatureThe reaction mixture was refluxed for 4 hrs
- concentrationwas concentrated to a residue on a rotary evaporator
- additionWater and ethyl acetate were added
- customThe organic phase was separated
- washwashed with saturated sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- filtrationAfter filtration
- customthe solvent was evaporated to dryness
출처 및 근거
- ORD 기록
- ord-4915d56f036b428187c79fe574ec5742
- 출처 데이터셋
- uspto-grants-1993_11
- 특허 번호
- US05266567
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