反応 #50006

反応方程式

calcium carbonate

7-amino-2,4-dichloro-6-fluorobenzothiazole

thiophosgene

→

2,4-Dichloro-6-fluoro-7-isothiocyanatobenzothiazole

溶媒

water

dichloromethane

dichloromethane

反応条件

後処理

1. 1
   ろ過The solid was filtered
2. 2
   その他the phases were separated
3. 3
   乾燥the organic phase dried over magnesium sulfate
4. 4
   濃縮concentrated
5. 5
   その他The residue was purified by column chromatography (eluent: hexane/ethyl acetate)

実験手順

A suspension of 16.9 g calcium carbonate in 100 ml water was added to a solution of 19.4 g thiophosgene in 100 ml dichloromethane. A solution of 40 g 7-amino-2,4-dichloro-6-fluorobenzothiazole in 500 ml dichloromethane was added, dropwise at 5° C., and the mixture stirred for 8 hours at room temperature. The solid was filtered, the phases were separated, and the organic phase dried over magnesium sulfate and concentrated. The residue was purified by column chromatography (eluent: hexane/ethyl acetate). Yield: 16 g=38% of theory m.p.: 80°-81° C.

出典