反应详情

温度

85 °C

To a solution of the product (480 mg, 2.18 mmol) from Step A in ethanol (12 mL) was added chloroacetaldehyde (50 wt. % in water, 0.336 mL) and the mixture was heated at 85° C. for 3 h. After cooling to room temperature, the solution was concentrated under reduced pressure. The residue was partitioned between saturated aqueous sodium bicarbonate solution and dichloromethane. The organic phase was separated, dried (magnesium sulfate) and concentrated in vacuo to yield the product as light-brown solid which was used without further purification. LC/MS 244.8 (M+1).

1. temperatureAfter cooling to room temperature
2. concentrationthe solution was concentrated under reduced pressure
3. customThe residue was partitioned between saturated aqueous sodium bicarbonate solution and dichloromethane
4. customThe organic phase was separated
5. dry with materialdried (magnesium sulfate)
6. concentrationconcentrated in vacuo