Реакция #8949

ord-054a943755054727b3a0598de364fa67

Растворители

Условия реакции

Температура
110°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеto prepare a treating agent solution
  2. 2
    workup.ADDITIONtreated
  3. 3
    Промывкаwashed with water
  4. 4
    Другоеdried
  5. 5
    Другоеto uniformly absorb the total amount of the above treating agent solution
  6. 6
    Другоеair-dried for 3 hours at room temperature
  7. 7
    workup.ADDITIONThe dried cloth was heat-treated for 20 minutes at 140° C. in a batch type hot air oven (“IPHH-2000”, an inert oven manufactured by Tabaiesbeck Co., Ltd.)
  8. 8
    Промывкаwashed with water
  9. 9
    ПромывкаIt was further washed with 5% aqueous sodium bicarbonate solution
  10. 10
    Промывкаrinsed three times with water
  11. 11
    Промывкаsubsequently washed with 10% aqueous succinic acid solution
  12. 12
    Промывкаrinsed three times with water
  13. 13
    Промывкаfinally washed with household
  14. 14
    Промывкаwashing detergent solution
  15. 15
    Промывкаrinsed with water
  16. 16
    Другоеair-dried

Методика

2.33 Grams (10 mmol) of L-lysine methyl ester dihydrochloride, 1.11 g (3.1 mmol) of disodium phosphate 12 hydrate and 0.1 g of polyoxyethylene lauryl ether (“Newcol 1100”, nonionic surfactant produced by Nippon Nyukazai Co., Ltd.) were dissolved in 5.0 ml of water to prepare a treating agent solution. A cotton cloth (150 mm×170 mm, 4.8 g) was in advance treated to be immersed in 25% aqueous sodium hydroxide solution for an hour at room temperature, washed with water and dried. This treated cotton cloth was allowed to uniformly absorb the total amount of the above treating agent solution and then air-dried for 3 hours at room temperature. The dried cloth was heat-treated for 20 minutes at 140° C. in a batch type hot air oven (“IPHH-2000”, an inert oven manufactured by Tabaiesbeck Co., Ltd.) and washed with water. It was further washed with 5% aqueous sodium bicarbonate solution and rinsed three times with water and subsequently washed with 10% aqueous succinic acid solution and rinsed three times with water, and finally washed with household washing detergent solution, rinsed with water and air-dried. The identification of L-lysine cellulose ester was conducted by the following method. A part of the cloth was cut and a solution of ninhydrin in butanol was sprayed on it. Thereafter, it was heated for 10 minutes in an oven of 110° C. to cause coloring thereby the presence of the amino acid was confirmed. Also, a part of the cloth was cut and subjected to an infrared spectroscopic analysis whereby there was confirmed a peak based on ester bond at 1730–1750 cm−1. As a result of determination for the amount of the L-lysine bonded, it was 0.19 mmol based on 1 g of the cloth. The degree of esterfication was 0.031. Also, the amount of succinic acid was 0.39 mmol.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07091221B2uspto-grants-2006_08