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N,N-Diethylethylenediamine → N'-[2-(Diethylamino)ethyl]-N-(1-methylethyl)-N-[4-(phenylsulfonyl)butyl]urea hydrate

HRID 4229
ノート
印刷プレビュー

反応式

HRID 4229 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][CH:22]([NH:24][CH2:25][CH2:26][CH2:27][CH2:28][S:29]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)(=[O:31])=[O:30])[CH3:23]>O1CCCC1.C(Cl)(Cl)Cl>[OH2:2].[CH2:13]([N:15]([CH2:19][CH3:20])[CH2:16][CH2:17][NH:18][C:1](=[O:2])[N:24]([CH:22]([CH3:21])[CH3:23])[CH2:25][CH2:26][CH2:27][CH2:28][S:29]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)(=[O:30])=[O:31])[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

6

反応物 3

HCID 60993N,N-DiethylethylenediamineHCID 682631,1'-CarbonyldiimidazoleHCID 13655072N-(1-methylethyl)-4-(phenylsulfonyl]-1-butylamine

生成物 1

HCID 20152850N'-[2-(Diethylamino)ethyl]-N-(1-methylethyl)-N-[4-(phenylsulfonyl)butyl]urea hydrate収率 69.8%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒
HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

A solution of 1,1'-carbonyldiimidazole (6.00 g, 0.037 mole) and N,N-diethylethylenediamine (4.00 g, 0.034 mole) was stirred at room temperature for 2 hours in 200 ml of tetrahydrofuran. A solution of N-(1-methylethyl)-4-(phenylsulfonyl]-1-butylamine (free base 7.99 g, 0.0313 mole) in 100 ml of tetrahydrofuran was added and the solution was heated overnight at reflux. The reaction was stripped to dryness and the residue dissolved in chloroform. The chloroform was extracted with water, dried (sodium sulfate), filtered, and removed in vacuo. A dark brown oil was obtained upon removal of chloroform. This oil was subjected to flash chromatography on Silica Gel using 0.1N ammonium hydroxide-methanol for elution. This chromatography furnished 5.37 g (42.2% yield) of clear oil after drying in vacuo 18 hours at 60° C.

後処理

  1. temperaturethe solution was heated overnight
  2. temperatureat reflux
  3. extractionThe chloroform was extracted with water
  4. dry with materialdried (sodium sulfate)
  5. filtrationfiltered
  6. customremoved in vacuo
  7. customA dark brown oil was obtained upon removal of chloroform
  8. washThis oil was subjected to flash chromatography on Silica Gel using 0.1N ammonium hydroxide-methanol for elution

出典と根拠

ORDレコード
ord-f4da05c15f66425caadd5d8639eb6bb2
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04724235

反応ノート

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