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Ethylenediamine → N-[3-(4,5-dihydro-1H-imidazol-2-ylmethoxy)phenyl]methanesulfonamide hydrochloride

HRID 1106712
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반응식

HRID 1106712 반응식
[ClH:1].C(O[C:5](=[NH:19])[CH2:6][O:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])[CH:9]=1)C.[CH2:20](N)[CH2:21][NH2:22]>CO>[ClH:1].[NH:22]1[CH2:21][CH2:20][N:19]=[C:5]1[CH2:6][O:7][C:8]1[CH:9]=[C:10]([NH:14][S:15]([CH3:18])(=[O:16])=[O:17])[CH:11]=[CH:12][CH:13]=1
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참가 물질

4

반응물 2

HCID 3301EthylenediamineHCID 69351950HCID 69351950, 화합물

생성물 1

HCID 18789725N-[3-(4,5-dihydro-1H-imidazol-2-ylmethoxy)phenyl]methanesulfonamide hydrochloride수율 20.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

2-(3-Methanesulfonylaminophenoxy)-acetimidic acid ethyl ester hydrochloride (0.8 g) was suspended in 12 ml of absolute methanol (MeOH) and treated with 0.16 g of ethylene diamine. After 8 hours at room temperature the solvent was evaporated. The residue was purified by silica gel chromatography eluting with methanol:dichloromethane:ammonium hydroxide (16:84:0.1). Conversion to the hydrochloride salt by addition of 1.0M hydrogen chloride in ether gave 0.16 g of N-[3-(4,5-dihydro-1H-imidazol-2-ylmethoxy) phenyl] methanesulfonamide hydrochloride, mp 183-187° C.

후처리

  1. customAfter 8 hours at room temperature the solvent was evaporated
  2. customThe residue was purified by silica gel chromatography
  3. washeluting with methanol:dichloromethane:ammonium hydroxide (16:84:0.1)
  4. additionConversion to the hydrochloride salt by addition of 1.0M hydrogen chloride in ether

출처 및 근거

ORD 기록
ord-c7cf42a84feb4fda8c78f85cee4b7c7b
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06057349

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