Reaktion #155724

Reaktionsgleichung

n-butyl bromide

Intermediate c

2-phenyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile

DMF

NaH

→

Intermediate f

Ausbeute 81.4%

2-phenyl-4-butyl-3,5-dioxo-2,3,4,5-tetrahydro-1,2,4-triazine-6-carbonitrile

Ausbeute 81.4%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONAfter the dropwise addition
2. 2
   workup.WAITthe reaction was conducted at 70° C. for 6 h
3. 3
   SonstigeAfter completion of the reaction
4. 4
   SonstigeA great deal of solid separated out
5. 5
   Filtrationwas filtered by suction
6. 6
   WaschenThe filtered cake was washed with water
7. 7
   Sonstigedried

Vorschrift

Intermediate c (9 g, 0.042 mol) was added to DMF (100 mL). To the mixture was added NaH (1.3 g, 0.054 mol) in batch under an ice bath. After stirring for 30 min, n-butyl bromide (3.4 mL, 0.042 mol) was added dropwise. After the dropwise addition, the reaction was conducted at 70° C. for 6 h. After completion of the reaction, the reaction solution was poured into water (600 mL). A great deal of solid separated out and was filtered by suction. The filtered cake was washed with water and dried to produce Intermediate f (8.2 g) in a yield of 81.4%.

Quelle