Hydrochloric Acid → HCID 12134604, compound

Participants

Reaction Conditions

Reaction Steps

To 13% (v/v) NaOCl (140 ml, purchased from Fluka) solution was added the titled compound of Example 2 (12.85 g, 0.0578 mol), followed by stirring. After being refluxed for 30 min while maintaining the temperature of 65° C., the reaction mixture was cooled down to a room temperature, stirred for 30 min and filtered to obtain a filtrate. To the said filtrate was added 10 ml of 25% (w/v) sodium hydrosulfide, and then, concentrated hydrochloric acid was added to adjust the pH by 3-4. The reaction mixture was filtered to give a solid, which was then washed and recrystallized with a mixture of water and ethanol (40:60, v/v) to prepare the titled compound (6.262 g, 48%, m.p. 119-123° C.).

Provenance & Evidence