Reaktion #993680

Reaktionsgleichung

methyl iodide

3-(2,4-dimethylphenyl)-1,6-dimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one

compound 101

3-(2,4-dimethylphenyl)-1,6-dimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one

NaH

→

expected product

3-(2,4-Dimethylphenyl)-1,6,9-trimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture is stirred at AT for 18 hours
2. 2
   SonstigeIt is evaporated to dryness
3. 3
   Waschenthe organic phase is washed with NaCl
4. 4
   Trocknenwater, dried
5. 5
   Sonstigeevaporated
6. 6
   Filtrationfiltration
7. 7
   Sonstigedrying

Vorschrift

400 mg of 3-(2,4-dimethylphenyl)-1,6-dimethyl-1,9-dihydro-2H-pyrido[2,3-b]indol-2-one (compound 101) are dissolved in 10 ml of DMF. 31 mg of 95% NaH are added and the mixture is stirred at AT for 30 minutes. 380 μl of methyl iodide are added and the mixture is stirred at AT for 18 hours. It is evaporated to dryness. The residue is taken up in CH2Cl2 and the organic phase is washed with NaCl and then water, dried and evaporated. The residue is taken up in Et2O, filtration is carried out and drying is carried out. 300 mg of the expected product are obtained, M.p.=150° C.

Quelle