反応 #170754

反応方程式

2-(tert-butyldimethylsilanyloxymethyl)-2-propen-1-ol

2,4-dimethoxybenzylamine

methanesulfonyl chloride

triethylamine

triethylamine

→

titled compound

[2-(tert-Butyldimethylsilanyloxymethyl)allyl]-(2,4-dimethoxybenzyl)amine

溶媒

chloroform

water

反応条件

後処理

1. 1
   その他at 0° C.
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 15 hours
3. 3
   その他an organic layer was separated from the mixture
4. 4
   濃縮concentrated under reduced pressure
5. 5
   その他The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1)

実験手順

To a solution of 2-(tert-butyldimethylsilanyloxymethyl)-2-propen-1-ol (1.58 g) in chloroform (16 ml) were sequentially added triethylamine (2.2 ml) and methanesulfonyl chloride (0.73 ml) at 0° C., and then the mixture was stirred for 2 hours. To this reaction solution were sequentially added triethylamine (1.2 ml) and 2,4-dimethoxybenzylamine (1.3 ml), and then the mixture was stirred at room temperature for 15 hours. To this reaction mixture was added water, and an organic layer was separated from the mixture, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=1/1) to give the titled compound (1.14 g).

出典