Dimethylformamide → 2,6-Dichloroimidazo[1,2-a]pyridine-3-carbaldehyde

温度

0 °C

Compound 12 (1.0 g, 5.4 mmol) was dissolved in DMF (5 mL) and the solution cooled to 0° C.in an ice-water bath. To this solution was added POCl3 (0.6 mL, 6.4 mmol) and the mixture stirred for 15 min. The bath was removed and the mixture warmed to room temperature and stirred for 3 hours. This reaction mixture was poured into ice water. The aqueous suspension was made basic by the addition of concentrated NH4OH and the precipitated solid collected by filtration. This solid was dissolved in CHCl3 (50 mL) and the solution extracted with water (3×50 mL), dried (MgSO4) and solvent removed under reduced pressure to give 1.0 g (87%) of compound 50 as a white solid.

1. customThe bath was removed
2. temperaturethe mixture warmed to room temperature
3. stirringstirred for 3 hours
4. additionThis reaction mixture was poured into ice water
5. additionThe aqueous suspension was made basic by the addition of concentrated NH4OH
6. filtrationthe precipitated solid collected by filtration
7. dissolutionThis solid was dissolved in CHCl3 (50 mL)
8. extractionthe solution extracted with water (3×50 mL)
9. dry with materialdried (MgSO4) and solvent
10. customremoved under reduced pressure

ORDレコード

ord-7216569bf3c94fa78938f2ad674e9f96

出典データセット

uspto-grants-2001_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06214801B1