تفاعل #607474

ord-8a1ea0f3bdd44598bdefa03f3c68ff30

معادلة التفاعل

CC(C)(C)OC(=O)C(CN)(CN)C(=O)OC(C)(C)C.O=C(O)CCC1CC(CCCC2CCN(CCC(=O)O)C(CCC(=O)O)C2)CCN1CCC(=O)O
4,4′-trimethylene dipiperidine bispropanoic acid bis-boc-1,3-diamino propane
Cl
HCl
NCCCN.O=C(O)CCC1CC(CCCC2CCN(CCC(=O)O)C(CCC(=O)O)C2)CCN1CCC(=O)O
product
المردود 122.7%
NCCCN.O=C(O)CCC1CC(CCCC2CCN(CCC(=O)O)C(CCC(=O)O)C2)CCN1CCC(=O)O
4,4′-trimethylene dipiperidine bispropanoic acid 1,3-diamino propane
المردود 122.7%

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter removal of the solvent under reduced pressure
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in 10 mL of methanol/water (1:1)
  3. 3
    workup.ADDITIONwas treated with 5 g of Amberlyst OH 26 resin
  4. 4
    workup.STIRRINGAfter stirring at room temperature for 3 hours
  5. 5
    ترشيحthe resin was filtered off
  6. 6
    أخرىThe filtrate was evaporated dryness

الإجراء التجريبي

To 0.55 g of 4,4′-trimethylene dipiperidine bispropanoic acid-bis-boc-1,3-diamino propane dissolved in 5 mL of methanol was added 0.5 mL of concentrated HCl and the reaction mixture was stirred at 50° C. for 10 hours. After removal of the solvent under reduced pressure, the residue was dissolved in 10 mL of methanol/water (1:1) and was treated with 5 g of Amberlyst OH 26 resin. After stirring at room temperature for 3 hours, the resin was filtered off. The filtrate was evaporated dryness and the residue was lyophilized yielding 0.5 g of the product as a white solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09326994B2uspto-grants-2016_05