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1-Chlorodecane → Piperazine, 1-decyl-4-methyl-

HRID 1438836
ノート
印刷プレビュー

反応式

HRID 1438836 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[CH2:8](Cl)[CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].[OH-].[Na+]>O.C(O)C(C)C>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[CH2:4][CH2:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 138481-ChlorodecaneHCID 14798Sodium HydroxideHCID 531671-Methylpiperazine

生成物 1

HCID 11776460Piperazine, 1-decyl-4-methyl-収率 75%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6560Isobutanol溶媒

反応条件

温度
150 °C

実験手順

100 g (1 mole) of 1-methyl-piperazine and 176.5 g (1 mole) of decyl chloride were heated under reflux, at an external temperature of 150° C, until the reaction mixture had ceased boiling. After cooling, the solid product was extracted by shaking with a mixture with 40 g (1 mole) of sodium hydroxide in 500 ml of water and 500 ml of isobutanol. The organic phase was separated off and concentrated, and the residue was extracted with petroleum ether. After evaporating the petroleum ether solution, 180 g (75% of theory) of 1-methyl-4-decyl-piperazine were obtained in a form which was pure according to thin layer chromatography.

後処理

  1. temperatureAfter cooling
  2. extractionthe solid product was extracted
  3. customThe organic phase was separated off
  4. concentrationconcentrated
  5. extractionthe residue was extracted with petroleum ether
  6. customAfter evaporating the petroleum ether solution

出典と根拠

ORDレコード
ord-6561f23eefa645af89901cbd6e127488
出典データセット
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04057413

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート