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Potassium Carbonate → 1-[2-(N,N-dimethylamino)-4-nitrophenoxy]-2-[N-(3,4-dimethoxyphenethyl)-N-methylamino]ethane

HRID 1106882
ノート
印刷プレビュー

反応式

HRID 1106882 の反応式
Cl[CH2:2][CH2:3][N:4]([CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([O:16][CH3:17])[CH:9]=1)[CH3:5].[CH3:18][N:19]([C:21]1[CH:26]=[C:25]([N+:27]([O-:29])=[O:28])[CH:24]=[CH:23][C:22]=1[OH:30])[CH3:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.C(=O)(O)[O-].[Na+]>[CH3:20][N:19]([C:21]1[CH:26]=[C:25]([N+:27]([O-:29])=[O:28])[CH:24]=[CH:23][C:22]=1[O:30][CH2:2][CH2:3][N:4]([CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[C:10]([O:16][CH3:17])[CH:9]=1)[CH3:5])[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 136051471-chloro-2-[N-(3,4-dimethoxyphenethyl)-N-methylamino]ethaneHCID 187899052-(N,N-dimethylamino)-4-nitrophenol

生成物 1

HCID 187898891-[2-(N,N-dimethylamino)-4-nitrophenoxy]-2-[N-(3,4-dimethoxyphenethyl)-N-methylamino]ethane収率 55.6%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide
溶媒
HCID 516892Sodium Bicarbonate溶媒

実験手順

A portion (1 g, 3.88 mmol) of the 1-chloro-2-[N-(3,4-dimethoxyphenethyl)-N-methylamino]ethane produced in (1) above, 2-(N,N-dimethylamino)-4-nitrophenol (0.598 g, 3.88 mmol) and potassium carbonate (0.536 g, 3.88 mmol) were heated in dimethylformamide (10 ml) at 80° C. for 2 h. Thereafter, the reaction mixture was diluted with a saturated solution of sodium bicarbonate, subjected to extraction with ethyl acetate and dried with anhydrous magnesium sulfate, followed by evaporation of the solvent. The residue was purified by being subjected to column chromatography on silica gel using, as an eluent, chloroform containing methanol (5%) to yield the titled compound 1-[2-(N,N-dimethylamino)-4-nitrophenoxy]-2-[N-(3,4-dimethoxyphenethyl)-N-methylamino]ethane (0.87 g) as a foam.

後処理

  1. extractionsubjected to extraction with ethyl acetate
  2. dry with materialdried with anhydrous magnesium sulfate
  3. customfollowed by evaporation of the solvent
  4. customThe residue was purified
  5. additionchloroform containing methanol (5%)

出典と根拠

ORDレコード
ord-29c84e0e96ec45e590972983251fbe69
出典データセット
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06057358

反応ノート

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