Hydrochloric Acid → HCID 58193743, compound
Reaction equation
CO[C:3]([C:5]1([C:9]#[N:10])[CH2:8][CH2:7][CH2:6]1)=[O:4].CO.[CH2:13]([NH2:16])[CH2:14][NH2:15].Cl>O>[NH2:15][CH2:14][CH2:13][NH:16][C:3]([C:5]1([C:9]#[N:10])[CH2:8][CH2:7][CH2:6]1)=[O:4]Participants
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
8.74 g (0.063 mol) of 4 and 50 mL of methanol were mixed, after which the mixture was added dropwisely into 3.77 g (4.25 mL) of ethylene diamine to form a reaction solution. The reaction solution was subjected to reaction at room temperature for 15 hours, followed by evaporation to obtain yellow oil. The yellow oil was stirred with water and was mixed with HCl to adjust pH to 2 to obtain a crude product. The crude product was purified by placing in a column (3×20 cm) filled with 100 mL of AG 50 W×8 cationic exchange resin and elutriating with water and HCl solution having gradient concentrations, collecting an eluent fraction of a gradient concentration from 0.5 N to 1.0 N, and followed by evaporating the eluent fraction to obtain 6.37 g (0.038 mol, 60.49%) of 5.
Workup
- customto form a reaction solution
- customThe reaction solution was subjected to reaction at room temperature for 15 hours
- customfollowed by evaporation
- customto obtain yellow oil
- customto obtain a crude product
- customThe crude product was purified
- additionfilled with 100 mL of AG 50 W×8 cationic exchange resin
- concentrationgradient concentrations
- customcollecting
- concentrationan eluent fraction of a gradient concentration from 0.5 N to 1.0 N
- customby evaporating the eluent fraction
Sources & evidence
- ORD record
- ord-8f239b632c104893b0d01703d0e69635
- Source dataset
- uspto-grants-2013_01
- Patent number
- US08354512B2
Reaction notes
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