반응 #1106668

ord-1a12c87f41054061aa0a5b8452b10717

반응 방정식

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
수율 38.8%
CN(C)CCNc1cccc2c1C(=O)c1cccc(NCCO)c1C2=O
1-(2-(dimethylamino)ethylamino)-5-(2-hydroxyl ethylamino)anthracene-9,10-dione
수율 38.8%

용매

반응 조건

온도
-150°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was cooled to room temperature
  2. 2
    추출extracted with water and brine
  3. 3
    건조The organic layer was dried (Na2SO4)
  4. 4
    기타evaporated

실험 절차

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:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08715944B2uspto-grants-2014_05