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N,N-Diethylethylenediamine → N'-[2-(Diethylamino)ethyl]-N-[2-[(4-methoxyphenyl)sulfonyl]ethyl]-N-(1-methylethyl)urea

HRID 745185
ノート
印刷プレビュー

反応式

HRID 745185 の反応式
[C:1](N1C=CN=C1)(N1C=CN=C1)=[O:2].[CH2:13]([N:15]([CH2:19][CH3:20])[CH2:16][CH2:17][NH2:18])[CH3:14].[CH3:21][O:22][C:23]1[CH:28]=[CH:27][C:26]([S:29]([CH2:32][CH2:33][NH:34][CH:35]([CH3:37])[CH3:36])(=[O:31])=[O:30])=[CH:25][CH:24]=1>O1CCCC1>[CH2:13]([N:15]([CH2:19][CH3:20])[CH2:16][CH2:17][NH:18][C:1](=[O:2])[N:34]([CH2:33][CH2:32][S:29]([C:26]1[CH:25]=[CH:24][C:23]([O:22][CH3:21])=[CH:28][CH:27]=1)(=[O:30])=[O:31])[CH:35]([CH3:37])[CH3:36])[CH3:14]
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 60993N,N-DiethylethylenediamineHCID 682631,1'-CarbonyldiimidazoleHCID 13655063N-[2-[(4-methoxyphenyl)sulfonyl]ethyl]-2-propanamine

生成物 1

HCID 13655132N'-[2-(Diethylamino)ethyl]-N-[2-[(4-methoxyphenyl)sulfonyl]ethyl]-N-(1-methylethyl)urea収率 67.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 4.54 g (0.28 mole) of 1,1'-carbonyldiimidazole and 2.90 g (0.025 mole) of N,N-diethylethylenediamine in 400 ml of tetrahydrofuran was stirred at room temperature for 1 hr. A solution of 5.89 g (0.0229 mole) of N-[2-[(4-methoxyphenyl)sulfonyl]ethyl]-2-propanamine in 50 ml of tetrahydrofuran was added, and the mixture was refluxed overnight. The solvent was removed in vacuo, and the residue was dissolved in 800 ml of a 50/50 mixture of methylene chloride-ether. The organic solution was extracted with water and was dried over magnesium sulfate. The solvent was removed in vacuo to give an oil. This was crystallized from ether-hexane to give 6.16 g (67.3%) of white crystalline solid; m.p. 39.5°-42° C.

後処理

  1. temperaturethe mixture was refluxed overnight
  2. customThe solvent was removed in vacuo
  3. dissolutionthe residue was dissolved in 800 ml of a 50/50 mixture of methylene chloride-ether
  4. extractionThe organic solution was extracted with water
  5. dry with materialwas dried over magnesium sulfate
  6. customThe solvent was removed in vacuo
  7. customto give an oil
  8. customThis was crystallized from ether-hexane

出典と根拠

ORDレコード
ord-a29eb7ba9c72433b820584ea8117e843
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04597902

反応ノート

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