反应 #2314303

ord-c4632cad514544f4bf5ee4ce400e90ce

反应方程式

N[C@@H](Cc1ccc(O)cc1)C(=O)O
tyrosine
O=S1(=O)CCCC1
tetramethylene sulfone
N[C@@H](CCC(=O)O)C(=O)O
glutamic acid
N[C@@H](Cc1ccccc1)C(=O)O
phenylalanine
N[C@@H](CC(=O)O)C(=O)O
aspartic acid
N[C@@H](CC(=O)O)C(=O)O.N[C@@H](CCC(=O)O)C(=O)O.N[C@@H](Cc1ccc(O)cc1)C(=O)O.N[C@@H](Cc1ccccc1)C(=O)O
Glu Asp Tyr Phe

溶剂

反应条件

温度
190°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture was heated for one-half hour
  2. 2
    温度the mixture heated at 190° C. for 3 hours
  3. 3
    温度the mixture heated at 190° C. for 1.5 hours
  4. 4
    workup.STIRRINGAfter stirring for about 1 hour
  5. 5
    过滤the mixture was filtered
  6. 6
    过滤filtered
  7. 7
    其他The pH of the slurry (at 25° C.)
  8. 8
    过滤The mixture was filtered
  9. 9
    洗涤the cake washed with a small amount of water
  10. 10
    其他evaporated to dryness in vacuo

实验过程

750 ml of tetramethylene sulfone was heated to 190° C. in an inert nitrogen atmosphere in a 4 liter flask with stirring. 294 g of glutamic acid was added and the mixture was heated for one-half hour. 266 g of aspartic acid was added and the mixture heated as rapidly as possible to 190° C. and held there for 15 minutes. 362 g of tyrosine was added and the mixture heated at 190° C. for 3 hours. 330 g of phenylalanine was added and the mixture heated at 190° C. for 1.5 hours. The hot melt was then poured into 5 liters of water with vigorous stirring. After stirring for about 1 hour, the mixture was filtered and the filtrate discarded. The cake was reslurried in 5 liters of water, filtered and the cake was again reslurried in 5 liters of water. The pH of the slurry (at 25° C.) was adjusted to 8 using 40% sodium hydroxide solution. The mixture was filtered and the cake washed with a small amount of water. The washes and filtrate are combined and evaporated to dryness in vacuo to give Glu/Asp/Tyr/Phe proteinoid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06413550B1uspto-grants-2002_07