반응식
C([N:3]([CH2:6][CH3:7])[CH2:4]C)C.CN.C(Cl)C=[CH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>CO>[CH2:6]([NH:3][CH3:4])[CH:7]=[CH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1참가 물질
실험 절차
Triethylamine (0.66 g; 6.55 mmol) was added to 40% solution of methylamine in methanol (20 ml). While the mixture was stirred at room temperature, cinnamyl chloride (1.00 g; 6.55 mmol) was added dropwise. After completion of the addition, the mixture was stirred for 20 hours at room temperature, and excess methylamine and methanol were removed under reduced pressure. The residue was taken up in a mixture of diethyl ether and 2N hydrochloric acid (100 ml-100 ml), and the aqueous layer was neutralized with aqueous sodium hydroxide solution, followed by extraction with chloroform (100 ml). The organic layer was washed with saturated aqueous sodium bicarbonate solution and then with saturated brine, and dried over sodium sulfate. The solvent was evaporated under reduced pressure, to thereby yield 0.80 g of the target compound as yellow oily matter (yield: 83.0%).
후처리
- additionAfter completion of the addition
- stirringthe mixture was stirred for 20 hours at room temperature
- customexcess methylamine and methanol were removed under reduced pressure
- additionThe residue was taken up in a mixture of diethyl ether and 2N hydrochloric acid (100 ml-100 ml)
- extractionfollowed by extraction with chloroform (100 ml)
- washThe organic layer was washed with saturated aqueous sodium bicarbonate solution
- dry with materialwith saturated brine, and dried over sodium sulfate
- customThe solvent was evaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-6ccf9d5ec7cd452e89cc8c4b5df5ac97
- 출처 데이터셋
- uspto-grants-2003_07
- 특허 번호
- US06586633B1
연결된 노트
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