Hydrogen Peroxide → HCID 178483450, 화합물

HRID 25617

반응식

HRID 25617 반응식
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

참가 물질

7

반응물 5

HCID 784Hydrogen PeroxideHCID 1176UreaHCID 6811Phthalic AnhydrideHCID 11430Potassium CarbonateHCID 178483449HCID 178483449, 화합물

생성물 1

HCID 178483450HCID 178483450, 화합물수율 63%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3dc8f3bc5c254208a25af1057fbd914b
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858651B2

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