反应 #1561220

ord-9547a76e43dc488cb3b91aa3c4fac3aa

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture was heated
  2. 2
    其他was removed
  3. 3
    温度continue refluxing for half an hour
  4. 4
    其他After most of solvent was removed
  5. 5
    过滤the solid was filtered
  6. 6
    洗涤washed with 20% ethanol aqueous solution
  7. 7
    其他dried

实验过程

Phenylguanidine carbonate (13.5 g, 100 mmol), β-keto esters (22.3 g, 120 mmol) and 120 mL of toluene were added to 250 mL of flask in sequence, the mixture was heated to reflux with a Dean Stark trap until all the water was removed, and continue refluxing for half an hour. After most of solvent was removed, the reaction solution was cooled to room temperature, the solid was filtered, washed with 20% ethanol aqueous solution and dried to obtain 18.3 g of white solid (II-1) with yield of 71.2%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09018218B2uspto-grants-2015_04