تفاعل #3499

معادلة التفاعل

water

sodium hydride

methyl N-methoxycarbamate

chloromethylpropargyl ether

→

methyl N-methoxy-N-propargyloxymethylcarbamate

المردود 75.9%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةin this order while being cooled with ice
2. 2
   درجة الحرارةThe mixture was heat-refluxed for 1 hour
3. 3
   workup.ADDITIONwas added to the reaction solution
4. 4
   استخلاصthe mixture was extracted with ethyl acetate
5. 5
   أخرىThe extract was dried
6. 6
   تركيزconcentrated
7. 7
   أخرىpurified by silica gel column chromatography

الإجراء التجريبي

0.37 g of sodium hydride (60% in oil) was suspended in 10 ml of tetrahydrofuran, and 0.8 g of methyl N-methoxycarbamate and 0.96 g of chloromethylpropargyl ether were added thereto in this order while being cooled with ice. The mixture was heat-refluxed for 1 hour. After completion of the reaction, water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The extract was dried, concentrated and purified by silica gel column chromatography to obtain 1.0 g of methyl N-methoxy-N-propargyloxymethylcarbamate.

المصدر