Hydrochloric Acid → HCID 67303272, compound

Participants

Reaction Conditions

Reaction Steps

To a 250 mL three necked round bottomed flask, added iron powder (1.99 grams, 6.81 mmol) and 10 mL of demineralized water. Stirred the mass for 5 minutes and added concentrated hydrochloric acid (12 mL) drop-wise. The reaction was exothermic. Further, heated the reaction mass to 50° C. and added a solution of 2-methoxy-5-nitro-N-methyl-N-(1-methyl piperidin-4-yl)phenylamine (1.9 grams, 6.81 mmol) obtained at step (IV) was dissolved in ethanol (20 mL), drop-wise through addition funnel. The reaction mass was heated at 78-80° C. for 4 hours. After completion of reaction (thin layer chromatography), ethanol was distilled off completely under reduced pressure to obtain oily mass. Added water (50 mL) and basified to pH: 9 using 50% aqueous sodium hydroxide solution. Filtered the inorganic and washed the cake with ethyl acetate (2×50 mL). The organic layer was separated and dried over anhydrous sodium sulfate and concentrated to obtain 2.31 grams of oily product.

Provenance & Evidence