反応 #595348

反応方程式

water

sodium hydride

[2-(4-chlorophenyl)-1,3-oxazol-4-yl]methanol

chlorodimethyl ether

→

2-(4-Chlorophenyl)-4-[(methoxymethoxy)methyl]-1,3-oxazole

溶媒

THF

反応条件

後処理

1. 1
   workup.WAITat RT for 1 h
2. 2
   温度The reaction mixture is again cooled to 0° C.
3. 3
   workup.STIRRINGThe mixture is stirred at 0° C. for 10 min
4. 4
   workup.WAITat RT for 2 h
5. 5
   抽出the reaction mixture is extracted three times with in each case 25 ml of ethyl acetate
6. 6
   乾燥The combined organic phases are dried over magnesium sulfate
7. 7
   その他the solvent is removed on a rotary evaporator
8. 8
   その他The product obtained
9. 9
   その他is used without further purification in the subsequent reaction

実験手順

1.32 g (7.54 mmol) of [2-(4-chlorophenyl)-1,3-oxazol-4-yl]methanol (Example 100A) are initially charged in 18.5 ml of dry THF and cooled to 0° C., and 0.33 g (8.29 mmol) sodium hydride (60% strength in mineral oil) are added. The mixture is stirred at 0° C. for 10 min and then at RT for 1 h. The reaction mixture is again cooled to 0° C., and 0.69 ml (9.04 mmol) of chlorodimethyl ether is added. The mixture is stirred at 0° C. for 10 min and then at RT for 2 h. 5 ml of water are then added, and the reaction mixture is extracted three times with in each case 25 ml of ethyl acetate. The combined organic phases are dried over magnesium sulfate and the solvent is removed on a rotary evaporator. The product obtained is used without further purification in the subsequent reaction.

出典