تفاعل #3498

ord-cf112f9f981e4357be02e4ddbd112b54

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwhile being cooled with ice
  2. 2
    درجة الحرارةThe mixture was heat-refluxed for 4 hours
  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

0.43 g of sodium hydride (60% in oil) was suspended in 10 ml of tetrahydrofuran, and 1.0 g of methyl N-methoxycarbamate and 1.36 g of propargyl bromide were added to the suspension in this order while being cooled with ice. The mixture was heat-refluxed for 4 hours. 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 0.8 g of methyl N-methoxy-N-propargylcarbamate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733935uspto-grants-1998_03