反应 #8894

反应方程式

product

1-[3-Amino-5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)furo[2,3-b]pyridin-2-yl]-2,2-dimethylpropan-1-one

4-chlorobutyryl chloride

triethylamine

→

title compound

4-Chloro-N-[5-(4-chlorophenyl)-6-(2,4-dichlorophenyl)-2-(2,2-dimethylpropanoyl)furo[2,3-b]pyridin-3-yl]butanamide

溶剂

CH2Cl2

反应条件

后处理

1. 1
   其他The reaction mixture was then partitioned between saturated aqueous NaHCO3 and EtOAc
2. 2
   其他The organic layer was separated
3. 3
   洗涤washed with aq. NaHCO3, brine
4. 4
   干燥dried (Na2SO4)
5. 5
   过滤filtered
6. 6
   其他evaporated
7. 7
   其他The residue was purified on a silica gel flash chromatography column
8. 8
   洗涤eluted with 0–20% EtOAc-hexane
9. 9
   其他Evaporation of the purified fractions
10. 10
    其他drying in vacuo

实验过程

To a magnetically stirred solution of 0.300 g (0.63 mmol) of the product of Example 17 in 6 mL of CH2Cl2 at 0° C. was added 70 μL (0.63 mmol) of 4-chlorobutyryl chloride and 96 mg (0.95 mmol) of triethylamine. The reaction was stirred for 1.5 h and allowed to warm to room temperature. The reaction mixture was then partitioned between saturated aqueous NaHCO3 and EtOAc. The organic layer was separated, washed with aq. NaHCO3, brine, then dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–20% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the title compound. HPLC/MS: 577.0 (M+1), 578.9 (M+3); Rt=5.05 min.

来源