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

HRID 326539
ノート
印刷プレビュー

反応式

HRID 326539 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5cee5c73faa44083adc47af4d2f203ac
出典データセット
uspto-grants-1993_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05270310

反応ノート

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