反应 #657275

ord-476249cbcfe6473cb8c58188d6000e04

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The solution was filtered
  2. 2
    其他the 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
    过滤After filtration
  6. 6
    其他the solution was evaporated in vacuo to dryness
  7. 7
    其他the product was recrystallised from ethyl acetate

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09023656B2uspto-grants-2015_05