반응 #2267051

ord-b049ff2f73d042a3b35a2fdc9e87e9f6

용매

반응 조건

온도
20°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타to form an admixture
  2. 2
    기타After evaporation
  3. 3
    추출extracted with ethyl acetate
  4. 4
    건조The extract was dried over Na2SO4
  5. 5
    기타evaporated again
  6. 6
    workup.STIRRINGthe resultant BOC-Gly-D-Arg-Gly-Asp-Phe-Val-OH (SEQ ID NO 2) was stirred at 20 C for 2 hours with 20 ml of 2 N HCl in dioxane
  7. 7
    기타The resultant admixture was evaporated

실험 절차

Two grams (g) of BOC-Gly-D-Arg-Gly-Asp-Phe-Val-OMe (SEQ ID NO 1) were first dissolved in 60 milliliters (ml) of methanol to which was added 1.5 ml of 2 N sodium hydroxide solution to form an admixture. The admixture was then stirred for 3 hours at 20 degrees C (20 C). After evaporation, the residue was taken up in water, acidified to pH 3 with diluted HCl and extracted with ethyl acetate. The extract was dried over Na2SO4, evaporated again and the resultant BOC-Gly-D-Arg-Gly-Asp-Phe-Val-OH (SEQ ID NO 2) was stirred at 20 C for 2 hours with 20 ml of 2 N HCl in dioxane. The resultant admixture was evaporated to obtain H-Gly-D-Arg-Gly-Asp-Phe-Val-OH (SEQ ID NO 3) that was subsequently dissolved in a mixture of 1800 ml of dichloromethane and 200 ml of dimethylformamide (DMF) followed by cooling to 0 C. Thereafter, 0.5 g of dicyclohexylcarbodiimide (DCCl), 0.3 g of 1-hydroxybenzotriazole (HOBt) and 0.23 ml of N-methylmorpholine were added successively with stirring.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06887473B1uspto-grants-2005_05