反应详情

温度

0 °C

A solution of 3.0 grams of disulfide acid from Example 76 in 50 mL of tetrahydrofuran was cooled in an ice bath. A 2.1 mL portion of isobutyl chloroformate followed by a 1.8 mL portion of N-methyl morpholine were added. After stirring for 5 minutes at 0° C., 0.85 grams of 6-amino 4-(3-bromoanilino)quinazoline was added. The mixture was stirred for 3 hours at 0° C. and then allowed to warm to room temperature. The reaction was quenched with water and the tetrahydrofuran was evaporated under vacuum. Addition of methylene chloride followed by washing the methylene chloride layer with water and evaporation of the solvent gave a crude product. Silica gel chromatography with methanol in methylene chloride gave 0.15 grams white solid of product.

1. additionwere added
2. stirringThe mixture was stirred for 3 hours at 0° C.
3. temperatureto warm to room temperature
4. customThe reaction was quenched with water
5. customthe tetrahydrofuran was evaporated under vacuum
6. additionAddition of methylene chloride
7. washby washing the methylene chloride layer
8. customwith water and evaporation of the solvent
9. customgave a crude product