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Hydrochloric Acid → 2-Methyl-1-[3-(N-hexadecanoyl)aminopropyl]piperidine hydrochloride

HRID 326539
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반응식

HRID 326539 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][N:3]1[CH2:8][CH2:9][CH2:10][NH:11][C:12](=[O:28])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27].[ClH:29]>C(OCC)C>[ClH:29].[CH3:1][CH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][N:3]1[CH2:8][CH2:9][CH2:10][NH:11][C:12](=[O:28])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 197352342-methyl-1-[3-(N-hexadecanoyl)aminopropyl]piperidine

생성물 1

HCID 197352372-Methyl-1-[3-(N-hexadecanoyl)aminopropyl]piperidine hydrochloride수율 71%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a solution of 2-methyl-1-[3-(N-hexadecanoyl)aminopropyl]piperidine (0.47 g, 1.2 mmole) in diethyl ether was added an ethereal solution of hydrogen chloride. The reaction mixture was placed in the refrigerator overnight. The precipitate was filtered. The gummy paste was dissolved in methanol and the solvent removed under reduced pressure to give the title compound (0.37 g, 71%) as a pale paste. 1H NMR (300 MHz, CDCl3): mixture of rotamers, major peaks given. δ0.870 (H, t, J=6.7 Hz), 1.243 (24H, bs), 1.533 (3H, d, J=6.4 Hz), 1.59 to 1.66 (2H, m), 1.81 to 1.88 (2H, m), 2.06 to 2.70 (8H, m), 2.74 to 3.10 (2H, m), 3.12 to 3.70 (3H, m), and 7.264 (1H, bs). IR (neat): 2686, 1941, 1649, 1549, 1468, 1379, 1230, and 1123 cm-1. Analysis calculated for C25H51CIN2O.3/4H2O: C, 67.53; H, 11.90; N, 6.30; Cl, 7.97. Found: C, 67.55; H, 11.85; N, 6.29; Cl, 8.04.

후처리

  1. customwas placed in the refrigerator overnight
  2. filtrationThe precipitate was filtered
  3. dissolutionThe gummy paste was dissolved in methanol
  4. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-5cee5c73faa44083adc47af4d2f203ac
출처 데이터셋
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05270310

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