反応 #50426

ord-7dd6d28afe984fcabec32adca10aa985

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture then was cooled to room temperature during which a crystalline solid
  2. 2
    その他formed
  3. 3
    ろ過The crystals were filtered
  4. 4
    洗浄washed with isopropyl alcohol, ether
  5. 5
    その他dried in vacuo

実験手順

2-Di-n-propylamino-8-(1-oxo-3-(dimethylamino)-prop-2-enyl)-1,2,3,4-tetrahydronaphthalene, prepared as in Example 8 (0.18 g; 0.55 mmol) was dissolved in 3 ml of ethanol. To the mixture was added 0.07 g (1.1 mmol) of guanidine, and the mixture was stirred at 60° C. under nitrogen for 18 hours. The mixture then was cooled to room temperature during which a crystalline solid formed. The crystals were filtered, washed with isopropyl alcohol, ether, and dried in vacuo to give 70 mg of the title compound as glistening plates. The product was recrystallized from isopropyl alcohol to obtain colorless crystals, m.p. 188°-189° C. Analysis: Theory: C, 74.04; H, 8.70; N, 17.27; Found: C, 74.30; H, 8.70; N, 17.45.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05426226uspto-grants-1995_06