反应详情

Boron trichloride solution (1M in dichloromethane) was added to a suspension of 2-Amino-4-(5-benzyloxy-2,4-dichlorophenyl)-thieno[2,3-d]pyrimidine-6-carboxylic acid ethyl amide in dichloromethane, at −78° C. under a nitrogen atmosphere. The suspension was stirred for ˜3 hrs at room temperature. The suspension was cooled in ice and methanol added, the resulting mixture was stirred for ˜1 hr. and concentrated to a yellow green solid. The solids were suspended in aqueous sodium acetate (10%) and extracted with ethyl acetate. The extracts were washed with water and saturated aqueous sodium chloride solution. The solution was dried over anhydrous sodium sulphate and concentrated to a pale brown solid, washed with hexane dried in vacuo.

1. temperatureThe suspension was cooled in ice
2. stirringthe resulting mixture was stirred for ˜1 hr
3. concentrationand concentrated to a yellow green solid
4. extractionextracted with ethyl acetate
5. washThe extracts were washed with water and saturated aqueous sodium chloride solution
6. dry with materialThe solution was dried over anhydrous sodium sulphate
7. concentrationconcentrated to a pale brown solid
8. washwashed with hexane
9. customdried in vacuo