Hydrogen Peroxide → HCID 178483450、化合物

HRID 25617

反応式

HRID 25617 の反応式
OO.NC(N)=[O:5].C1(=O)OC(=O)C2=CC=CC=C12.[Cl:18][C:19]1[CH:24]=[CH:23][C:22]([O:25][C:26](=[O:44])[N:27]([C@H:29]2[CH2:34][CH2:33][C@H:32]([O:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][N:41]([CH3:43])[CH3:42])[CH2:31][CH2:30]2)[CH3:28])=[CH:21][CH:20]=1.C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl>[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([O:25][C:26](=[O:44])[N+:27]([O-:5])([C@H:29]2[CH2:34][CH2:33][C@H:32]([O:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][N:41]([CH3:42])[CH3:43])[CH2:31][CH2:30]2)[CH3:28])=[CH:23][CH:24]=1

参加物

7

反応物 5

HCID 784Hydrogen PeroxideHCID 1176UreaHCID 6811Phthalic AnhydrideHCID 11430Potassium CarbonateHCID 178483449HCID 178483449、化合物

生成物 1

HCID 178483450HCID 178483450、化合物収率 63%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of 1.39 g (4.4 mmol, 2.2 eq) Hydrogen peroxide.Urea adduct in CH2Cl2, 338.5 mg (2.2 mmol, 1.1 eq) phthalic anhydride were added and stirred for 15 min at RT. 800 mg (2.01 mmol) trans-[4-(5-Dimethylamino-pentyloxy)-cyclohexyl]-methyl-carbamic acid 4-chloro-phenyl ester in CH2Cl2 was added and the mixture was stirred at RT for 2 h. 5% aqueous K2CO3 solution was added and the inorganic phase was extracted with CH2Cl2. The organic phases were washed with water and brine and dried over MgSO4. Column chromatography yielded 525 mg (63%) trans-[4-(5-Dimethylamino-pentyloxy)-cyclohexyl]-methyl-carbamic acid 4-chloro-phenyl ester N-oxide as colourless oil, MS: 413 (MH+, 1Cl).

後処理

  1. stirringthe mixture was stirred at RT for 2 h
  2. extractionthe inorganic phase was extracted with CH2Cl2
  3. washThe organic phases were washed with water and brine
  4. dry with materialdried over MgSO4

出典と根拠

ORDレコード
ord-3dc8f3bc5c254208a25af1057fbd914b
出典データセット
uspto-grants-2005_02
特許番号
US06858651B2

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