Hydrochloric Acid → HCID 178518955、化合物

To a solution of 2-amino-5-bromobenzoic acid (50 g) in water (200 mL) was added HCl (46 mL). To the mixture was added aqueous NaNO2 solution (17.7 g/37 mL) at 0° C., and the mixture was stirred at 0° C. for 30 minutes. To the reaction solution was added dropwise aqueous Na2SO3 solution (79.3 g/200 mL) at 0° C., and the mixture was stirred at room temperature for 2 hours. To the mixture was added HCl (70 mL), and the mixture was stirred at room temperature for 18 hours and then at 80° C. for 4 hours. The precipitated solid was dissolved by basifying the reaction solution, and then the solution was acidified to precipitate a solid. The solid was collected by filtration and dried under reduced pressure to give Compound Q2 (36 g).

1. stirringthe mixture was stirred at room temperature for 2 hours
2. stirringthe mixture was stirred at room temperature for 18 hours
3. waitat 80° C. for 4 hours
4. dissolutionThe precipitated solid was dissolved
5. customto precipitate a solid
6. filtrationThe solid was collected by filtration
7. customdried under reduced pressure
8. customto give Compound Q2 (36 g)

ORDレコード

ord-dab41520d8b14460af7b8008d81434e2

出典データセット

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08765786B2