反应 #1985942

反应方程式

4-acetoxy-6-bromo-3-methoxybenzaldehyde

triethylamine

methyl acrylate

→

desired product

Methyl 5-Acetoxy-2-formyl-4-methoxycinnamate

溶剂

ether

water

DMF

反应条件

后处理

1. 1
   温度cooled to room temperature
2. 2
   洗涤The organic layer is washed with water, brine
3. 3
   干燥dried over magnesium sulfate
4. 4
   过滤filtered
5. 5
   浓缩concentrated in vacuo
6. 6
   其他The residue is purified by HPLC
7. 7
   洗涤eluting with 33% ethyl acetate in hexanes

实验过程

To a degassed solution of 4-acetoxy-6-bromo-3-methoxybenzaldehyde (15.4 g), and bis(triphenylphosphine)palladium (11) (1.2 g) in DMF (150 ml) is added triethylamine (31.9 ml) and methyl acrylate (19.6 g). The mixture is heated 135° C. for about 1.5 hours, cooled to room temperature and diluted with ether and water. The organic layer is washed with water, brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is purified by HPLC, eluting with 33% ethyl acetate in hexanes, then methylene chloride, to give the desired product.

来源