Ethylamine hydrochloride → 3-chloro-N-methylpropane-1-sulfonamide

3-Chloropropylsulfonyl chloride 1 (16.8 g, 94.9 mmol), ethylamine hydrochloride (13.5 g, 200 mmol), and potassium carbonate (27.6 g, 200 mmol) were sequentially added to ethyl acetate (500 ml). After the addition of N-benzyltrimethylammonium chloride (about 200 mg) to the mixture, the resultant mixture was stirred for 2 hours at room temperature and dried over anhydrous sodium sulfate. The mixture was filtered through a small amount of silica2 gel and the filtrate was concentrated in vacuo to give 12 g (74%) of crude N-methyl-3-chloropropylsulfonamide (intermediate 3b) as a pale yellow oil.

1. dry with materialdried over anhydrous sodium sulfate
2. filtrationThe mixture was filtered through a small amount of silica2 gel
3. concentrationthe filtrate was concentrated in vacuo

ORDレコード

ord-1dc486a91e0940dfbce95d7559656c2a

出典データセット

uspto-grants-2003_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06525081B1