Sodium Hydroxide → HCID 70298353, compound

Participants

Reaction Steps

A mixture of the above ester (2.20 g, 0.0044 mol) and 20% sodium hydroxide (2 ml) in ethanol (18 ml) was stirred at room temperature for 24 h and left standing for additional 24 h. Ethanol was evaporated in vacuo and the residue was dissolved in dichloromethane (300 ml). The resulting solution was acidified with acetic acid, washed with water (3×15 ml) and the organic phase was dried (MgSO4). The solvent was evaporated in vacuo, the residue (2.60 g) was dissolved in a mixture of ether and acetone (1:1, 20 ml) and the solution was made acidic with a solution of hydrogen chloride in ether. The solvents were evaporated in vacuo, the amorphous residue was twice dissolved in acetone (20 ml) and re-evaporated in vacuo. The solid was suspended in dry ether (100 ml) and stirred at room temperature for 3 h. The precipitate was filtered off and dried in vacuo, affording 1.85 g (82%) of the title compound.

Provenance & Evidence