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

HRID 36760

反応式

HRID 36760 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-5196aa637c7740218f9e817e1b948708
出典データセット
uspto-grants-1995_05
特許番号
US05416210

関連ノート

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