反応 #8894

反応方程式

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

溶媒

CH2Cl2

反応条件

後処理

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

実験手順

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.

出典