反応 #62935

反応方程式

tris(dimethylamino)methane

1,4-cyclohexanedione

hydrochloric acid

guanidine carbonate

→

5,6,7,8-tetrahydro-6-ketoquinazolin-2-amine

溶媒

toluene

toluene

methanol

反応条件

後処理

1. 1
   その他The resulting solution is evaporated in-vacuo
2. 2
   温度the mixture is refluxed for 16 hours
3. 3
   その他The solvent is evaporated
4. 4
   洗浄the yellow residue is washed with cold water
5. 5
   その他recrystallized from absolute ethanol

実験手順

A solution of tris(dimethylamino)methane, 25.0 g (172 mmol), in 100 ml toluene is added dropwise, under nitrogen, to a solution of the monoethylene ketal of 1,4-cyclohexanedione, 25.0 g (160 mmol), in 300 ml of toluene. The resulting solution is evaporated in-vacuo and the residue is dissolved in 600 ml of methanol along with 38.72 g (320 mmol) of guanidine carbonate. The pH of the solution is adjusted to 9 with 15% hydrochloric acid and the mixture is refluxed for 16 hours. The solvent is evaporated and the yellow residue is washed with cold water and recrystallized from absolute ethanol to yield 11.0 g of 5,6,7,8-tetrahydro-6-ketoquinazolin-2-amine, ethylene ketal as yellow prisms; mp 214°-217° C.

出典