반응 #595348

반응 방정식

water

sodium hydride

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

chlorodimethyl ether

→

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

용매

THF

반응 조건

후처리

1. 1
   workup.WAITat RT for 1 h
2. 2
   온도The 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
   추출the reaction mixture is extracted three times with in each case 25 ml of ethyl acetate
6. 6
   건조The combined organic phases are dried over magnesium sulfate
7. 7
   기타the solvent is removed on a rotary evaporator
8. 8
   기타The product obtained
9. 9
   기타is used without further purification in the subsequent reaction

실험 절차

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.

출처