Réaction #6315

ord-eadcefa2a05d42d58610fc3268716e7a

Équation de réaction

CSc1nc(=O)c2cnn3c2n1CC=C3c1cccc(C(F)(F)F)c1
5-(methylthio)-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one
CC(C)N
isopropylamine
CCO
ethanol
CCO
ethanol
CC(C)Nc1nc(=O)c2cnn3c2n1CC=C3c1cccc(C(F)(F)F)c1
desired product
Rendement 62.3%
CC(C)Nc1nc(=O)c2cnn3c2n1CC=C3c1cccc(C(F)(F)F)c1
5-[(1-Methylethyl)amino]-8-[3-(trifluoromethyl)-phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one
Rendement 62.3%

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureThe reaction mixture is heated on a steambath for 18 hours
  2. 2
    TempératureThe mixture is cooled to 10° C.
  3. 3
    FiltrationThe product is collected by filtration
  4. 4
    Lavagewashed with ethanol (2×20 ml)
  5. 5
    Autreair-dried

Mode opératoire

To a suspension of 5.0 g of 5-(methylthio)-8-[3-(trifluoromethyl)phenyl]-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one in 35 ml of acetic acid is added 2.64 g of isopropylamine. The reaction mixture is heated on a steambath for 18 hours. The resulting solution is cooled to room temperature and 17 ml of ethanol added. The mixture is cooled to 10° C. and 35 ml of ethanol and 20 g of ice added. The mixture is stirred for an additional 30 minutes at -10° C. The product is collected by filtration, washed with ethanol (2×20 ml) and air-dried to give 3.2 g (62.3%) of the desired product.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US05247086uspto-grants-1993_09