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

HRID 618206
ノート
印刷プレビュー

反応式

HRID 618206 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3301EthylenediamineHCID 69351950HCID 69351950、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-332c2664a5704071893491a2bbebf883
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05952362

反応ノート

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