HCID 86749375, compound → HCID 22419891, compound

2-amino-4-fluorobenzylsulfonate (11.0 g) was added to phosphorous oxychloride (100 ml) at 50° C. and the mixture was heated under reflux for 6 hours. The reaction mixture was concentrated in vacuo and the resulting grease was poured into ice-water mixture. A sodium hydroxide solution was added to the mixture at 0° C. until the mixture was basic. Insoluble material was filtered off and washed with water. The filtrate was treated with aqueous hydrochloric acid solution (pH=2.5). The crude product was separated by filtration. Ethyl acetate was added to the precipitate and the insoluble material was filtered off. The filtrate was concentrated in vacuo, to give 1,3-dihydro-6-fluoro-2,1-benzisothiazole 2,2-dioxide (3.2 g)

1. temperaturethe mixture was heated
2. temperatureunder reflux for 6 hours
3. concentrationThe reaction mixture was concentrated in vacuo
4. additionthe resulting grease was poured into ice-water mixture
5. additionA sodium hydroxide solution was added to the mixture at 0° C. until the mixture
6. filtrationInsoluble material was filtered off
7. washwashed with water
8. additionThe filtrate was treated with aqueous hydrochloric acid solution (pH=2.5)
9. customThe crude product was separated by filtration
10. additionEthyl acetate was added to the precipitate
11. filtrationthe insoluble material was filtered off
12. concentrationThe filtrate was concentrated in vacuo

ORD record

ord-c8638cc32d3a436d980a0d688c342463

Source dataset

uspto-grants-1996_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05504095