反応 #73500

反応方程式

dimethylamine

6-chloropyridine-3-sulfonyl chloride

→

6-chloro-N,N-dimethylpyridine-3-sulfonamide

収率 93.0%

溶媒

EtOAc

THF

THF

反応条件

後処理

1. 1
   workup.ADDITIONis added dropwise, at 0° C.
2. 2
   洗浄washed with water (2×40 mL) and brine (40 mL)
3. 3
   乾燥dried over Na2SO4
4. 4
   ろ過filtered
5. 5
   濃縮concentrated under reduced pressure

実験手順

To a mixture of 4.7 mL (9.43 mmol) of dimethylamine (2N in THF) and 2.6 mL (18.86 mmol) of TEA in 20 mL of THF is added dropwise, at 0° C., a solution of 2 g (9.43 mmol) of 6-chloropyridine-3-sulfonyl chloride (prepared according to patent WO 9840332) in 5 mL of THF. After stirring for 40 minutes at 0° C., the reaction medium is taken up in 40 mL of EtOAc, washed with water (2×40 mL) and brine (40 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. 1.93 g of 6-chloro-N,N-dimethylpyridine-3-sulfonamide are obtained in the form of a brown solid, which is used without further purification in the following step.

出典