Methylamine → N-methyl-3-phenylprop-2-en-1-amine

HRID 1356823

반응식

HRID 1356823 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]=1

참가 물질

5

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

  1. additionAfter completion of the addition
  2. stirringthe mixture was stirred for 20 hours at room temperature
  3. customexcess methylamine and methanol were removed under reduced pressure
  4. additionThe residue was taken up in a mixture of diethyl ether and 2N hydrochloric acid (100 ml-100 ml)
  5. extractionfollowed by extraction with chloroform (100 ml)
  6. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution
  7. dry with materialwith saturated brine, and dried over sodium sulfate
  8. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-6ccf9d5ec7cd452e89cc8c4b5df5ac97
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586633B1

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