Reacción #81821

ord-85aae3c011414557809e137dd866b50d

Ecuación de reacción

CCN1c2ncccc2C(=O)Nc2c(C)cc(Cl)nc21
2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one
OC1CCNC1
3-hydroxypyrrolidine
CCN1c2ncccc2C(=O)Nc2c(C)cc(N3CCC(O)C3)nc21
title compound
CCN1c2ncccc2C(=O)Nc2c(C)cc(N3CCC(O)C3)nc21
5,11-Dihydro-11-ethyl-2-(3-hydroxypyrrolidin-1-yl)-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one

Disolventes

Condiciones de reacción

Temperatura
170°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter cooling to room temperature the mixture
  2. 2
    Extracciónextracted with ethyl acetate
  3. 3
    LavadoThe organic phase was washed
  4. 4
    Otrodried
  5. 5
    Otroevaporated

Procedimiento

A suspension of the 2-chloro-5,11-dihydro-11-ethyl-4-methyl-6H-dipyrido[3,2-b:2',3'-e][1,4]diazepin-6-one (0.14 g) in 3-hydroxypyrrolidine (0.29 g) in an open test tube was heated at 170° C. for 30 minutes. After cooling to room temperature the mixture was diluted with water and extracted with ethyl acetate. The organic phase was washed, dried, and evaporated. Chromatography over silica gel with ethyl acetate gave the title compound, which crystallized from ethyl acetate. Yield, 0.12 g, m.p. 131°-134° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05620974uspto-grants-1997_04