تفاعل #1807213

معادلة التفاعل

2-amino-4-fluorobenzylsulfonate

→

1,3-dihydro-6-fluoro-2,1-benzisothiazole 2,2-dioxide

المردود 31.7%

المذيبات

phosphorous oxychloride

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةunder reflux for 6 hours
3. 3
   تركيزThe reaction mixture was concentrated in vacuo
4. 4
   workup.ADDITIONthe resulting grease was poured into ice-water mixture
5. 5
   workup.ADDITIONA sodium hydroxide solution was added to the mixture at 0° C. until the mixture
6. 6
   ترشيحInsoluble material was filtered off
7. 7
   غسيلwashed with water
8. 8
   workup.ADDITIONThe filtrate was treated with aqueous hydrochloric acid solution (pH=2.5)
9. 9
   أخرىThe crude product was separated by filtration
10. 10
    workup.ADDITIONEthyl acetate was added to the precipitate
11. 11
    ترشيحthe insoluble material was filtered off
12. 12
    تركيزThe filtrate was concentrated in vacuo

الإجراء التجريبي

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)

المصدر