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

HRID 352027
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HRID 352027 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][S:5](Cl)(=[O:7])=[O:6].Cl.[CH2:10]([NH2:12])C.C(=O)([O-])[O-].[K+].[K+]>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.C(OCC)(=O)C>[CH3:10][NH:12][S:5]([CH2:4][CH2:3][CH2:2][Cl:1])(=[O:7])=[O:6]
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참가 물질

6

반응물 3

HCID 11198Ethylamine hydrochlorideHCID 11430Potassium CarbonateHCID 154103-Chloropropanesulphonyl chloride

생성물 1

HCID 102412533-chloro-N-methylpropane-1-sulfonamide수율 74%

시약·촉매·용매 2

HCID 5963Benzyltrimethylammonium chloride촉매HCID 8857Ethyl Acetate
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실험 절차

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 silica 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.

후처리

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

출처 및 근거

ORD 기록
ord-90f0a7066fb64014b0743cd036393fb5
출처 데이터셋
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06743923B2

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