反应详情

A solution of 5-(4-methoxyphenyl)-1H-pyrazol-3-amine and diisopropylethylamine in 10 volumes of a 9:1 mixture of acetonitrile:DMF was cooled to −10° C. 5-Bromovaleryl chloride was added dropwise over a minimum of 3 hr at −10° C. The resulting solution was held at −10° C. until reaction completion, generally 2 hr. The reaction mixture was quenched with water. The product was isolated by filtration, washed with water, TBME and suction dried. The product-wet cake was purified by re-slurrying in TBME at 35° C. for a minimum of 2 hr. The yield was 70-80%.

1. customThe resulting solution was held at −10° C. until reaction completion, generally 2 hr
2. customThe reaction mixture was quenched with water
3. customThe product was isolated by filtration
4. washwashed with water, TBME and suction
5. customdried
6. customThe product-wet cake was purified by re-slurrying in TBME at 35° C. for a minimum of 2 hr