Triethylamine → hexadecyl N-(4-methylpiperadinyl)carbamate

HRID 398744

반응식

HRID 398744 반응식
[NH2:1][N:2]1[CH2:7][CH2:6][CH:5]([CH3:8])[CH2:4][CH2:3]1.C(N(CC)CC)C.Cl[C:17]([O:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])=[O:18]>C(Cl)(Cl)Cl>[CH3:8][CH:5]1[CH2:6][CH2:7][N:2]([NH:1][C:17](=[O:18])[O:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH3:35])[CH2:3][CH2:4]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 97633Cetyl chloroformateHCID 37335874-Methylpiperidin-1-amine

생성물 1

HCID 131720856hexadecyl N-(4-methylpiperadinyl)carbamate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

6.3 Grams of N-amino-4-methylpiperadine, 6.0 g of triethylamine and 120 ml of chloroform were charged in a flask equipped with a stirrer, a condenser and a calcium chloride drying tube and stirred with ice cooling. To the solution was slowly added dropwise 15.2 g of hexadecyl chloroformate. After completion of the addition, the temperature of the solution was returned to room temperature, followed by refluxing with heating for 0.5 hour. The reaction mixture was cooled to room temperature, washed with water, dried over anhydrous magnesium sulfate and, then, concentrated under reduced pressure. The residue was recrystallized from acetonitrile to obtain 16.8 g of the desired product. m.p. 92° C.

후처리

  1. customequipped with a stirrer, a condenser and a calcium chloride drying tube
  2. additionAfter completion of the addition
  3. customwas returned to room temperature
  4. temperatureby refluxing
  5. temperaturewith heating for 0.5 hour
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-b76e220b51e34a6095ee14f718de536d
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817599

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