反应 #1483126

ord-7c25bd8d1ac84b2f9b71eb142266dcbf

反应方程式

O=c1c(O)c(O)c1=O
squaric acid
CCCCOc1cccc(N(C)CCO)c1
2-(methyl(3-butoxyphenyl)amino)ethan-1-ol
CCCCO
n-BuOH
CCCCOc1cc(N(C)CCO)ccc1C1=C(O)C(c2ccc(N(C)CCO)cc2OCCCC)=C1O
desired compound
CCCCOc1cc(N(C)CCO)ccc1C1=C(O)C(c2ccc(N(C)CCO)cc2OCCCC)=C1O
2,4-bis(2-n-butoxy-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kept being reacted
  5. 5
    温度the reactant was cooled down
  6. 6
    其他producing crystals
  7. 7
    过滤The crystals was filtered
  8. 8
    洗涤several times washed with hexanes
  9. 9
    其他once more recrystallized

实验过程

342 mg of squaric acid and 2.14 g of 2-(methyl(3-butoxyphenyl)amino)ethan-1-ol was put in a 100 mL 3-necked round 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 7 hour. Then, a Dean-Stark trap set was used to remove water generated from the reactant during the reaction and kept being reacted. When the reaction was complete, the reactant was cooled down, producing crystals. The crystals was filtered, several times washed with hexanes, and once more recrystallized, obtaining a desired compound.

来源

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