تفاعل #334095

ord-be3c7ea898e04beda97c7de9a7faf593

معادلة التفاعل

O=C([O-])C(F)(F)F
trifluoroacetate
N=C(N)NCCC[C@H](N)C(=O)O
H-Arg
C[C@H](NC(=O)OC(C)(C)C)C(=O)O
Boc-Ala-OH
CN(C)[P+](On1nnc2ccccc21)(N(C)C)N(C)C.F[P-](F)(F)(F)(F)F
BOP
C[C@H](N)C(=O)N[C@@H](CCCNC(=N)N)C(=O)O
H-Ala-Arg

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe reaction is terminated after 4 hrs
  2. 2
    أخرىThe medium is evaporated to dryness in vacuo at 25°
  3. 3
    غسيلThe organic phase is washed with a 5% aqueous solution of NaHCO3, with water
  4. 4
    أخرىdried
  5. 5
    أخرىevaporated
  6. 6
    أخرىThe tripeptide is recrystallized in ethyl-acetate/ether
  7. 7
    أخرىfinally dried in vacuo

الإجراء التجريبي

443 g of trifluoroacetate of H-Arg (NO2) Leu-NH2 are dissolved in 2 l of DMF. 200 g of Boc-Ala-OH, then 500 g of BOP are added. The pH is adjusted to 7 with pH paper (on small samples of the reaction medium) with the aid of NEM. The medium is stirred and the development of the reaction is followed by TLC. The reaction is terminated after 4 hrs. The medium is evaporated to dryness in vacuo at 25°. The residue is taken up in 2 l of water and 2 l of ethyl acetate. The organic phase is washed with a 5% aqueous solution of NaHCO3, with water, dried and evaporated. The tripeptide is recrystallized in ethyl-acetate/ether, and finally dried in vacuo. It is monitored by TLC and NMR.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04704450uspto-grants-1987_11