反応 #605196

反応方程式

2,4-dichloro-6,7-dihydro-thieno[3,2-d]pyrimidin

diisopropylethylamine

(R)-(−)-2-amino-3-methyl-1-butanol

→

(R)-2-(2-chloro-6,7-dihydro-thieno[3,2-d]pyrimidin-4-ylamino)-3-methyl-butan-1-ol

溶媒

dioxane

反応条件

後処理

1. 1
   温度cooled
2. 2
   その他evaporated down
3. 3
   workup.ADDITIONThe residue is treated with petroleum ether/ethyl acetate 9:1 in the ultrasound bath
4. 4
   ろ過filtered
5. 5
   その他dried
6. 6
   その他8.3 g (III-2) are obtained as a solid

実験手順

7.2 g 2,4-dichloro-6,7-dihydro-thieno[3,2-d]pyrimidin (II) are placed in 36 ml dioxane, then 18 ml diisopropylethylamine and then 6.1 g (R)-(−)-2-amino-3-methyl-1-butanol are added. The reaction mixture is heated to 100° C. until no further reaction takes place, then cooled and evaporated down. The residue is treated with petroleum ether/ethyl acetate 9:1 in the ultrasound bath and the solid is suction filtered and dried. 8.3 g (III-2) are obtained as a solid. Analytical HPLC (method A): RT=2.75 min

出典