반응 #86598

반응 방정식

DIPEA

2-(3-(benzyloxycarbonylamino)-2-oxopyridin-1(2H)-yl)acetic acid

TBTU

HOBt

isopentylamine

→

Benzyl 1-(2-(isopentylamino)-2-oxoethyl)-2-oxo-1,2-dihydropyridin-3-ylcarbamate

용매

DMF

반응 조건

후처리

1. 1
   기타The solvent is removed in vacuo
2. 2
   세척subsequently washed with 10% citric acid (3×75 ml), saturated NaHCO3 solution (3×75 ml) and brine (75 mL)
3. 3
   건조The organic phase is dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated in vacuo in dryness
6. 6
   기타Brown solid is obtained
7. 7
   기타it is suitable for further processing without purification

실험 절차

A mixture of 900 mg of 2-(3-(benzyloxycarbonylamino)-2-oxopyridin-1(2H)-yl)acetic acid (˜2.32 mmol), 744 mg of TBTU (2.32 mmol), 313 mg of HOBt (2.32 mmol) is dissolved in 25 mL of DMF. By addition of 985 μL of DIPEA (5.79 mmol, 2.5 eq) a pH value is adjusted to ˜9. 539 μL of isopentylamine (4.63 mmol) is added and the mixture is stirred at RT for 2.5 h. The solvent is removed in vacuo and the obtained residue is taken up in 100 mL of DCM and subsequently washed with 10% citric acid (3×75 ml), saturated NaHCO3 solution (3×75 ml) and brine (75 mL). The organic phase is dried over Na2SO4, filtered and concentrated in vacuo in dryness. Brown solid is obtained and it is suitable for further processing without purification.

출처