反应详情

To a stirring mixture of 10.3 g (69.8 mmol) 4-chloro-thiazole-5-carbaldehyde (Journal of the Chemical Society, Perkins Transactions, 1992, 973-978), 296 ml (2792 mmol) 2-methyl-2-butene, and 200 mL tertiary butanol was added a solution of 50.5 g (558 mmol) NaClO2, 50.2 g (419 mmol) NaH2PO4 in 300 mL of water, dropwise over 20 minutes. The reaction was stirred for 1 hour then concentrated to 1/3 volume via rotary evaporation. The remaining solution was acidified with 6N HCl with rapid stirring. The precipitated solid was filtered and air dried under high vacuum overnight to give 10.6 g of white solid.

1. concentrationthen concentrated to 1/3 volume via rotary evaporation
2. filtrationThe precipitated solid was filtered
3. customair dried under high vacuum overnight