Reaktion #8952

ord-e1ae6626684141c2bc4822f377cdc2d6

Lösungsmittel

Reaktionsbedingungen

Temperatur
110°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeto prepare a treating agent solution
  2. 2
    workup.ADDITIONtreated
  3. 3
    Waschenwashed with water
  4. 4
    Sonstigedried
  5. 5
    Sonstigeto uniformly absorb the total amount of the above treating agent solution
  6. 6
    Sonstigeair-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
    Waschenwashed with water
  9. 9
    WaschenIt was further washed with 5% aqueous sodium bicarbonate solution
  10. 10
    Waschenrinsed three times with water
  11. 11
    Waschensubsequently was washed with 10% aqueous citric acid solution
  12. 12
    Waschenrinsed three times with water
  13. 13
    Waschenfinally washed with household
  14. 14
    Waschenwashing detergent solution
  15. 15
    Waschenrinsed with water
  16. 16
    Sonstigeair-dried

Vorschrift

2.33 Grams (10 mmol) of L-lysine methyl ester dihydrochloride was 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 was washed with 10% aqueous citric 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 1720–1740 cm1. As a result of determination for the amount of the L-lysine bonded, it was 0.10 mmol based on 1 g of the cloth. The degree of esterfication was 0.016.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07091221B2uspto-grants-2006_08