Piperidine → 11-(Piperidin-1-yl)undecan-1-ol

HRID 1886001ノート

反応式

HRID 1886001 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13].[NH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.Br.N1CCCCC1>>[OH:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][N:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

参加物

4

反応物 3

HCID 8082PiperidineHCID 7416311-Bromo-1-undecanolHCID 203244Piperidine, hydrobromide (1:1)

生成物 1

HCID 312228311-(Piperidin-1-yl)undecan-1-ol収率 96.3%

実験手順

11-Bromoundecanol (11.00 g., 43.79 mmole) was dissolved in 100 ml. of piperidine and heated at reflux temperature for 18 hours. The reaction mixture was allowed to cool and most of the precipitated piperidine hydrobromide was removed by filtration. The excess piperidine is removed by simple distillation and the resultant solid residue is recrystallized from ethanol and water. After drying, 10.78 g. (96.3% yield) of 1-hydroxy-11-(N-piperidyl)undecane was obtained . m.p. 62°-65° C., 1H-NMR (200 MHz, CDCl3) δ=1.2-1.7 ppm, m, 24H; 2.10, broad s, 1H; 2.20-2.45, m, 6H; 3.63, t, 2H.

後処理

  1. temperatureat reflux temperature for 18 hours
  2. customwas removed by filtration
  3. customThe excess piperidine is removed by simple distillation
  4. customthe resultant solid residue is recrystallized from ethanol and water
  5. customAfter drying

出典と根拠

ORDレコード
ord-41723e7074b44283811eb5dd0fb97725
出典データセット
uspto-grants-1992_09
特許番号
US05149524

反応ノート

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