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Pyridine → N-(6-Acetoxyhexyl)-N-methylaniline

HRID 414434
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HRID 414434 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH3:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[C:16](OC(=O)C)(=[O:18])[CH3:17].N1C=CC=CC=1>>[C:16]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH3:15])[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)(=[O:18])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 152539786-[Methyl(phenyl)amino]hexan-1-OL

생성물 1

HCID 19697246N-(6-Acetoxyhexyl)-N-methylaniline

실험 절차

A mixture of 210 g (1.01 mol) of N-(6-hydroxyhexyl)-N-methylaniline, 112 g (1.10 mol) of acetic anhydride, and 86 g (1.1 mol) of pyridine was heated at reflux with stirring for 2 hours. After cooling, the solution was poured onto 500 g of ice and extracted with ethyl acetate (4×300 mL). The combined extracts were dried (MgSO4) and the solvent was removed at reduced pressure. The residue was distilled in vacuo, collecting the fraction boiling at 130° C. (0.01 mm). Yield: 231 g (93%) of a colorless oil.

후처리

  1. temperaturewas heated
temperature
at reflux
  • temperatureAfter cooling
  • extractionextracted with ethyl acetate (4×300 mL)
  • dry with materialThe combined extracts were dried (MgSO4)
  • customthe solvent was removed at reduced pressure
  • distillationThe residue was distilled in vacuo
  • customcollecting the fraction boiling at 130° C. (0.01 mm)
  • 출처 및 근거

    ORD 기록
    ord-adeca062cbeb4f8394c293cdee07a499
    출처 데이터셋
    uspto-grants-1988_12
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04792208

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