反应 #86598

反应方程式

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

溶剂

DMF

反应条件

后处理

1. 1
   其他The solvent is removed in vacuo
2. 2
   洗涤subsequently washed with 10% citric acid (3×75 ml), saturated NaHCO3 solution (3×75 ml) and brine (75 mL)
3. 3
   干燥The organic phase is dried over Na2SO4
4. 4
   过滤filtered
5. 5
   浓缩concentrated in vacuo in dryness
6. 6
   其他Brown solid is obtained
7. 7
   其他it is suitable for further processing without purification

实验过程

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.

来源