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

HRID 1438836
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반응식

HRID 1438836 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 138481-ChlorodecaneHCID 14798Sodium HydroxideHCID 531671-Methylpiperazine

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6560Isobutanol용매

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6561f23eefa645af89901cbd6e127488
출처 데이터셋
uspto-grants-1977_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04057413

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