反应 #1483125

ord-f20999db59ab4d6091d7d696ee33cec5

反应方程式

O=c1c(O)c(O)c1=O
squaric acid
CC(=O)Nc1cccc(N(C)CCO)c1
2-(methyl(3-acetaminophenyl)amino)ethan-1-ol
CCCCO
n-BuOH
CC(=O)Nc1cc(N(C)CCO)ccc1C1=C(O)C(c2ccc(N(C)CCO)cc2NC(C)=O)=C1O
desired compound
CC(=O)Nc1cc(N(C)CCO)ccc1C1=C(O)C(c2ccc(N(C)CCO)cc2NC(C)=O)=C1O
2,4-bis(2-acetamino-4-((2-hydroxyethyl)(methyl)amino)phenyl)cyclobuta-1,3-dien-1,3-diol

溶剂

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The mixture was heated
  2. 2
    其他to remove water
  3. 3
    其他generated from the reactant during the reaction
  4. 4
    其他the reactant kept being reacted
  5. 5
    温度the reactant was cooled down
  6. 6
    其他producing crystals
  7. 7
    过滤The crystals were filtered
  8. 8
    其他once more recrystallized

实验过程

342 mg of squaric acid) and 2 g of 2-(methyl(3-acetaminophenyl)amino)ethan-1-ol were put in a 100 mL 3-neck rounded bottom flask, and 40 mL of n-BuOH and 20 mL of toluene were added thereto. The mixture was heated and refluxed at 120° C. for 10 hours. Then, a Dean-Stark trap set was used to remove water generated from the reactant during the reaction, and the reactant kept being reacted. When the reaction was complete, the reactant was cooled down, producing crystals. The crystals were filtered, several times cleaned with hexane, and once more recrystallized, obtaining a desired compound.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08900780B2uspto-grants-2014_12