反応 #164523

反応方程式

benzotriazole

potassium carbonate

2-chloromethyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane

compound 7

2-chloromethyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane

→

2-(benzotriazol-1-yl)methyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane

溶媒

Dimethylformamide

DMF

反応条件

後処理

1. 1
   workup.ADDITIONAfter the addition, reaction mixture
2. 2
   温度maintained for 30 hrs
3. 3
   温度The reaction mixture was cooled to room temperature 28° C.
4. 4
   ろ過filtered
5. 5
   workup.DISTILLATIONThe solvent was distilled off
6. 6
   その他to get the product

実験手順

To 37.63 gm (0.3163 mole) of benzotriazole and 35 gm of potassium carbonate in Dimethylformamide (DMF) (350 ml) was added slowly under stirring 82 gm of 2-chloromethyl-8-(4,6-dimethoxy-pyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4,5]decane (intermediate for compound 7) in DMF (300 ml). After the addition, reaction mixture was heated to 120° C. and maintained for 30 hrs. The reaction mixture was cooled to room temperature 28° C. and filtered. The solvent was distilled off to get the product. It was a thick dark brown liquid. Yield of product was 90%

出典