反应详情

A solution of chloroacetic acid (30 g, 0.32 mol) in diethylamine (230 mL, 2.2 mol) was stirred overnight. The obtained white precipitate was removed by filtration. The filtrate was evaporated to dryness to afford yellow oil to which EtOAc (300 mL) was added. The obtained precipitate was again removed by filtration. The filtrate was evaporated to afford yellow solid residue (44 g) that was washed with hexane (2×100 mL), EtOAc (2×50 mL) and again with hexane (50 mL), and then dried in vacuo to afford title Intermediate 2 (38 g).

1. customThe obtained white precipitate was removed by filtration
2. customThe filtrate was evaporated to dryness
3. customto afford yellow oil to which EtOAc (300 mL)
4. additionwas added
5. customThe obtained precipitate was again removed by filtration
6. customThe filtrate was evaporated