反应详情

To a solution of benzhydrol (90 g, 0.488 mol) and trifluoroacetic acid (90 mL) in dichloromethane (300 mL) was added thioglycolic acid (40 g, 0.488 mol) in dichloromethane (60 mL) drop wise over 20 minutes. The reaction was completed in one hour. The solvent was removed in vacuo to give a crude solid, which was dried overnight under high vacuum. The solid was treated with 2 N NaOH (1.0 L) and washed with t-butylmethylether (200 ml) to remove non carboxylic acid impurities. The aqueous solution was then acidified with concentrated HCl and the resulting precipitate was collected, washed with water and dried to give benzhydrylthioacetic acid (128.5 g) as a colorless solid.

1. customThe solvent was removed in vacuo
2. customto give a crude solid, which
3. customwas dried overnight under high vacuum
4. additionThe solid was treated with 2 N NaOH (1.0 L)
5. washwashed with t-butylmethylether (200 ml)
6. customto remove non carboxylic acid impurities
7. customthe resulting precipitate was collected
8. washwashed with water
9. customdried