反应详情

温度

90 °C

A mixture prepared from 3.7 g of 3-chloro-7,8,9,10-tetrahydro-11H-pyrido[3',4':4,5]pyrrolo[2,3-c]quinoline, 0.45 g of paraformaladehyde and 100 ml of formic acid was heated at 90° C. for one hour. The reaction was quenched with water and the solution was made alkaline (pH9) with a sodium hydroxide solution. The crystalline product was filtered, washed with water and purified by HPLC using dichloromethane/methanol=8:2 as an eluent. Clean fractions were combined and concentrated, and the crystalline residue was stirred in isopropanol and filtered. The yield was 2.1 g, mp=286°-287° C.

1. customThe reaction was quenched with water
2. filtrationThe crystalline product was filtered
3. washwashed with water
4. custompurified by HPLC
5. concentrationconcentrated
6. filtrationfiltered