反応 #1106668

ord-1a12c87f41054061aa0a5b8452b10717

反応方程式

CN(C)CCNc1cccc2c1C(=O)c1cccc(Cl)c1C2=O
Compound 17
CN(C)CCNc1cccc2c1C(=O)c1cccc(Cl)c1C2=O
1-Chloro-5-(2-(dimethylamino)ethylamino)anthracene-9,10-dione
NCCO
ethanolamine
CN(C)CCNc1cccc2c1C(=O)c1cccc(NCCO)c1C2=O
Compound 21
収率 38.8%
CN(C)CCNc1cccc2c1C(=O)c1cccc(NCCO)c1C2=O
1-(2-(dimethylamino)ethylamino)-5-(2-hydroxyl ethylamino)anthracene-9,10-dione
収率 38.8%

溶媒

反応条件

温度
-150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled to room temperature
  2. 2
    抽出extracted with water and brine
  3. 3
    乾燥The organic layer was dried (Na2SO4)
  4. 4
    その他evaporated

実験手順

A mixture of Compound 17 (0.87 g, 2.7 mmol) and ethanolamine (0.8 mL, 13.23 mmol) was heated in an oil bath (−150° C.) for 18 hours. The mixture was cooled to room temperature, dissolved in 100 mL CH2Cl2 and extracted with water and brine. The organic layer was dried (Na2SO4) and evaporated to provide Compound 21 (370 mg). This product was used in the next step without any purification. Rf (9:1 CHCl3/MeOH) 0.19. The structure of Compound 21 is given below:

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08715944B2uspto-grants-2014_05