反应详情

To a stirring solution of trifluoroacetone (7.75 g, 69.2 mmol) in diethyl ether (60 ml) at −40° C. was added 4-methoxybenzyl amine (9.49 g, 69.2 mmol) and triethylamine (14 g, 138 mmol) in diethyl ether (40 ml). A cooled (0° C.) mixture of TiCl4 (6.56 g, 34.6 mmol) in hexane (40 ml) at was added dropwise over 10 minutes and the resulting mixture was allowed to warm up to ambient temperature over 20 mins and stirred at 50° C. for 2.5 h. The inorganic precipitate was removed by filtration and washed with diethyl ether. The filtrate was concentrated in vacuo to afford a yellow oil. Purification of the crude product by chromatography on silica eluting with 0% to 25% EtOAc in iso-hexane afforded the title product.

1. temperatureA cooled
2. additionat was added dropwise over 10 minutes
3. customThe inorganic precipitate was removed by filtration
4. washwashed with diethyl ether
5. concentrationThe filtrate was concentrated in vacuo
6. customto afford a yellow oil
7. customPurification of the crude product by chromatography on silica eluting with 0% to 25% EtOAc in iso-hexane