반응 #9966

반응 방정식

6-Amino-5-fluoro-2-methylbenzoxazole

sulfuryl chloride

→

6-Amino-7-Chloro-5-Fluoro-2-Methylbenzoxazole

용매

ethyl acetate

ethyl acetate

methylene chloride

methylene chloride

반응 조건

후처리

1. 1
   workup.ADDITIONcontaining
2. 2
   기타dry pryidine (5.8 mL, 72.22 mMole)
3. 3
   세척washed with 2N-HCl
4. 4
   건조dried (MgSO4)
5. 5
   여과filtered
6. 6
   농축concentrated
7. 7
   기타to give a solid
8. 8
   기타to give the product

실험 절차

6-Amino-5-fluoro-2-methylbenzoxazole (12 g, 72.22 mMole) was dissolved in ethyl acetate (100 mL) containing dry pryidine (5.8 mL, 72.22 mMole). At room temperature and with good stirring, sulfuryl chloride (7.0 mL, 86.66 mMole) was added drop by drop over a 20-minute period. After stirring at room temperature for about 30 minutes, the reaction was diluted with ethyl acetate, washed with 2N-HCl, dried (MgSO4), filtered and concentrated to give a solid. This solid was dissolved in methylene chloride and passed through a short column of silica gel eluting with methylene chloride to give the product. Yield 5.0 g.

출처