Water → 3,9-Bis(3-diethylaminopropoxy)-fluoranthene

HRID 268514노트

반응식

HRID 268514 반응식
O.[OH-].[Na+].[OH:4][C:5]1[CH:6]=[CH:7][C:8]2[C:9]3[C:14]([C:15]4[C:20]=2[C:19]=1[CH:18]=[CH:17][CH:16]=4)=[CH:13][CH:12]=[C:11]([OH:21])[CH:10]=3.Cl.[CH2:23]([N:25]([CH2:30][CH3:31])[CH2:26][CH2:27][CH2:28]Cl)[CH3:24]>C1(C)C=CC=CC=1>[CH2:23]([N:25]([CH2:30][CH3:31])[CH2:26][CH2:27][CH2:28][O:4][C:5]1[CH:6]=[CH:7][C:8]2[C:9]3[C:14]([C:15]4[C:20]=2[C:19]=1[CH:18]=[CH:17][CH:16]=4)=[CH:13][CH:12]=[C:11]([O:21][CH2:28][CH2:27][CH2:26][N:25]([CH2:30][CH3:31])[CH2:23][CH3:24])[CH:10]=3)[CH3:24]

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 145749Diethylaminopropyl chloride, hydrochlorideHCID 12546984Fluoranthene-3,9-diol

생성물 1

HCID 5156993,9-Bis(3-diethylaminopropoxy)-fluoranthene

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To 200 ml of water containing 16.0 g (0.4 mole) of sodium hydroxide and 15.7 g (0.067 mole) of 3,9-dihydroxyfluoranthene are added 200 ml of toluene and 27.9 g (0.15 mole) of 3-diethylaminopropyl chloride hydrochloride, and the heterogeneous reaction mixture is stirred at reflux for 24 hours. After cooling, the organic layer is washed with water, dried over magnesium sulfate, and concentrated in vacuo. The residue is crystallized from ether to give 3,9-bis(3-diethylaminopropoxy)-fluoranthene which is converted to the dihydrochloride salt with ethereal HCl and recrystallized from methanolbutanone, M.P. 235°-236.5°C.

후처리

  1. temperatureat reflux for 24 hours
  2. temperatureAfter cooling
  3. washthe organic layer is washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue is crystallized from ether

출처 및 근거

ORD 기록
ord-de1847eeaf9f4aa68a4db630a5126d85
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947593

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