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Hydrochloric Acid → 2,2'-[[(4-formylbenzyl)imino]bis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide)

HRID 445234
ノート
印刷プレビュー

反応式

HRID 445234 の反応式
C([O:3][CH:4](OCC)[C:5]1[CH:36]=[CH:35][C:8]([CH2:9][N:10]([CH2:23][C:24]2[N:25]([S:29]([N:32]([CH3:34])[CH3:33])(=[O:31])=[O:30])[CH:26]=[CH:27][N:28]=2)[CH2:11][C:12]2[N:13]([S:17]([N:20]([CH3:22])[CH3:21])(=[O:19])=[O:18])[CH:14]=[CH:15][N:16]=2)=[CH:7][CH:6]=1)C.Cl.C(=O)([O-])[O-].[Na+].[Na+]>C(OCC)(=O)C>[CH:4]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][N:10]([CH2:23][C:24]2[N:25]([S:29]([N:32]([CH3:34])[CH3:33])(=[O:31])=[O:30])[CH:26]=[CH:27][N:28]=2)[CH2:11][C:12]2[N:13]([S:17]([N:20]([CH3:22])[CH3:21])(=[O:18])=[O:19])[CH:14]=[CH:15][N:16]=2)=[CH:35][CH:36]=1)=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 672847312,2'-[{[4-(diethoxymethyl)benzyl]imino}bis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide)

生成物 1

HCID 866644642,2'-[[(4-formylbenzyl)imino]bis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide)収率 85.5%

試薬・触媒・溶媒 1

HCID 8857
Ethyl Acetate
溶媒

実験手順

2,2′-[{[4-(diethoxymethyl)benzyl]imino}bis(methylene)]bis(N,N-dimethyl-1H-imidazole-1-sulfonamide) (International Publication WO 2007/058322 pamphlet, Example 27; 10.0 g), ethyl acetate (100 mL) and 2N hydrochloric acid (100 mL) were added, followed by stirring at room temperature for 3 minutes. The aqueous layer was neutralized with an aqueous saturated sodium carbonate solution, extracted with ethyl acetate and then washed with saturated brine. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain the title compound (7.46 g) having the following physical properties.

後処理

  1. extractionextracted with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f0f0ba4e27d44f08a1c62eb52b8461e3
出典データセット
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08476290B2

反応ノート

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