تفاعل #657275

ord-476249cbcfe6473cb8c58188d6000e04

معادلة التفاعل

CC1CCCC(C)N1CC(=O)NCC(=O)O
[2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid
O=C1CCC(=O)N1O
N-Hydroxysuccinimide
C(=NC1CCCCC1)=NC1CCCCC1
N,N′-Dicyclohexyl-carbodiimide
CC1CCCC(C)N1CC(=O)NCC(=O)ON1C(=O)CCC1=O
[2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid-(2,5-dioxo-pyrrolidine-1-yl)-ester

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe solution was filtered
  2. 2
    أخرىthe filtrate was evaporated in vacuo to dryness
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in 50 mL dichloromethane
  4. 4
    workup.ADDITIONtreated with charcoal
  5. 5
    ترشيحAfter filtration
  6. 6
    أخرىthe solution was evaporated in vacuo to dryness
  7. 7
    أخرىthe product was recrystallised from ethyl acetate

الإجراء التجريبي

4.54 g (20 mMol) [2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid (30) were added to 2.30 g (20 mMol) N-Hydroxysuccinimide and 4.12 g (20 mMol) N,N′-Dicyclohexyl-carbodiimide dissolved in 150 ml dichloromethane. The reaction mixture was stirred for 16 h at room temperature. The solution was filtered and the filtrate was evaporated in vacuo to dryness. The residue was dissolved in 50 mL dichloromethane and treated with charcoal. After filtration, the solution was evaporated in vacuo to dryness and the product was recrystallised from ethyl acetate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09023656B2uspto-grants-2015_05