Hydrochloric Acid → 3-Bromo-4-fluorobenzenesulfonamide

温度

0 °C

A solution of 3-bromo-4-fluorobenzenesulfonyl chloride (1 g, 3.3 mmol, 90% pure) stirred at 0° C. in THF (15 ml) and DCM (5 ml) was treated with aqueous ammonium hydroxide (28%) by dropwise addition over 15 min. After stirring at 0° C. for 210 min, the mixture was acidified (pH=1) by addition of 1 N HCl (aq). After the mixture was concentrated in vacuo to near dryness, it was treated with water (50 ml), sonicated for 3 min and filtered. After the filter cake was washed sequentially with water (50 ml) and hexanes (100 ml), it was dried in vacuo to afford the title compound (503 mg, 60%) as a white solid which was carried forward without purification. LCMS (M−H)−=253.

1. concentrationAfter the mixture was concentrated in vacuo
2. additionwas treated with water (50 ml)
3. customsonicated for 3 min
4. filtrationfiltered
5. washAfter the filter cake was washed sequentially with water (50 ml) and hexanes (100 ml), it
6. customwas dried in vacuo

ORDレコード

ord-90881ee0511b4f7485bb610d8a5d70cd

出典データセット

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09115114B2