反応 #2275689

反応方程式

Triethylamine

Tris hydrochloride

2,2-dimethoxypropane

para-toluenesulfonic acid

→

product

収率 85.0%

(5-Amino-2,2-dimethyl-[1,3]dioxan-5-yl)-methanol

収率 85.0%

溶媒

DMF

反応条件

後処理

1. 1
   その他resulted
2. 2
   その他solvent evaporated
3. 3
   workup.DISSOLUTIONThe viscous crude was dissolved in triethylamine (40 ml)
4. 4
   workup.ADDITIONethyl acetate (750 ml) added
5. 5
   ろ過the white precipitate of ammonium salts was filtered off
6. 6
   workup.STIRRINGafter stirring for 30 mins
7. 7
   その他The filtrate was evaporated

実験手順

Tris hydrochloride (51 g, 324 mmol) was suspended in dry DMF (100 ml) and 2,2-dimethoxypropane (39 g, 374 mmol) was added followed by para-toluenesulfonic acid (2.6 g, 13.5 mmol). The mixture was stirred in a sealed flask for 18 h at ambient temperature when a clear solution resulted. Triethylamine (2.5 ml) was added and solvent evaporated. The viscous crude was dissolved in triethylamine (40 ml) and ethyl acetate (750 ml) added and the white precipitate of ammonium salts was filtered off after stirring for 30 mins. The filtrate was evaporated to give the product as a colourless liquid in approx. 85% yield.

出典