反応 #64879

反応方程式

phosgene

α-[2-chloro-4-fluoro-5-(4-methoxypyrazolidinyl-thiocarbonylamino)-phenylthio]-acetic acid methyl ester

→

desired product

8-(4-chloro-2-fluoro-5-methoxycarbonylmethylthio-phenyl-imino)-3-methoxy-7-thia-1,5-diazabicyclo[3.3.0]octan-6-one

溶媒

toluene

toluene

反応条件

後処理

1. 1
   洗浄the organic phase is washed with water
2. 2
   その他dried
3. 3
   濃縮concentrated
4. 4
   その他The product is purified by means of column chromatography

実験手順

At 0°-5° C., 4.2 ml of phosgene solution in toluene (20%) are added to a solution of 2.8 g of α-[2-chloro-4-fluoro-5-(4-methoxypyrazolidinyl-thiocarbonylamino)-phenylthio]-acetic acid methyl ester in 20 ml of toluene. After stirring for 2 hours at 22° C., the organic phase is washed with water, dried and concentrated. The product is purified by means of column chromatography to yield 2.21 g of the desired product, 8-(4-chloro-2-fluoro-5-methoxy-carbonylmethylthio-phenylimino)-3-methoxy-7-thia-1,5-diazabicyclo[3.3.0]octan-6-one, in the form of a yellow oil.

出典