반응 #73500

반응 방정식

dimethylamine

6-chloropyridine-3-sulfonyl chloride

→

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

수율 93.0%

용매

EtOAc

THF

THF

반응 조건

후처리

1. 1
   workup.ADDITIONis added dropwise, at 0° C.
2. 2
   세척washed with water (2×40 mL) and brine (40 mL)
3. 3
   건조dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated under reduced pressure

실험 절차

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.

출처