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

HRID 268514ノート

反応式

HRID 268514 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-de1847eeaf9f4aa68a4db630a5126d85
出典データセット
uspto-grants-1976_03
特許番号
US03947593

反応ノート

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