Propanamide, 3-amino-N-2-pyridinyl- synthesis
- Product Name:Propanamide, 3-amino-N-2-pyridinyl-
- CAS Number:774487-65-9
- Molecular formula:C8H11N3O
- Molecular Weight:165.19
Yield:774487-65-9 71.06%
Reaction Conditions:
Stage #1: 2-aminopyridine;3-(tert-butyloxycarbonylamino)propionic acidwith benzotriazol-1-ol;1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride in dichloromethane at 20; for 24 h;
Stage #2: with trifluoroacetic acid in dichloromethane at 20; for 0.5 h;
Steps:
10 Compound 3:
Add tert-butoxycarbonyl protected aminopropionic acid (22.68g, 120mmol) to dichloromethane (30ml),EDCI (25.3g, 132mmol), HOBt (17.82g, 132mmol) and 2-aminopyridine (12.42g, 132mmol) were added in sequence, and the reaction was stirred at room temperature for 24h.After the TLC detection reaction was completed, the solvent was removed under reduced pressure, and the resulting solid was redissolved in 120 mL of the mixed solution (DCM:TFA=7:3),After stirring the reaction at room temperature for 0.5h, the reaction was completed by TLC, and the solvent was removed by rotary evaporation under reduced pressure.The product compound 3 was isolated by column chromatography with a yield of 71.06% and HPLC: 99.67%.
References:
CN111233774,2020,A Location in patent:Paragraph 0201-0203
504-29-0
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