4-Methylmorpholine → HCID 22907047, 화합물

HRID 742044노트

반응식

HRID 742044 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([N:12]([CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:13]2([C:26](O)=[O:27])[CH2:18][CH2:17][N:16]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH2:15][CH2:14]2)(=[O:11])=[O:10])=[CH:5][CH:4]=1.CN1CCOCC1.Cl.[C:44]([O:48][NH2:49])([CH3:47])([CH3:46])[CH3:45].Cl.CN(CCCN=C=NCC)C>C(Cl)Cl.O>[C:44]([O:48][NH:49][C:26]([C:13]1([N:12]([S:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)(=[O:11])=[O:10])[CH2:29][C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:18][CH2:17][N:16]([CH2:19][C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH2:15][CH2:14]1)=[O:27])([CH3:47])([CH3:46])[CH3:45]

참가 물질

7

반응물 4

HCID 79724-MethylmorpholineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2777906O-tert-butylhydroxylamine hydrochlorideHCID 229072304-[[4-Methoxybenzenesulfonyl](benzyl)amino]-1-[benzyl]-4-[carboxy]piperidine

생성물 1

HCID 22907047HCID 22907047, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a mixture of 4-[[4-methoxybenzenesulfonyl](benzyl)amino]-1-[benzyl]-4-[carboxy]-piperidine (850.0 mg, 1.64 mmol) in methylene chloride (100 mL) containing N-methylmorpholine (0.6 ml, 5.48 mmol) and O-t-butylhydroxyl amine hydrochloride (620.0 mg, 4.94 mmol) is added N-[dimethylaminopropyl]-N'-ethylcarbodiimide hydrochloride (1.1 g, 5.74 mmol). The reaction mixture is stirred overnight at room temperature. The mixture is diluted with water and extracted with methylene chloride. The combined organic extracts are dried (Na2SO4) and the solvent is evaporated. The crude product is purified by silica gel chromatography (ethyl acetate) to provide 4-[N-t-butyloxy-carbamoyl]-4-[[4-methoxybenzenesulfonyl](benzyl)amino]-1-[benzyl]-piperidine.

후처리

  1. extractionextracted with methylene chloride
  2. dry with materialThe combined organic extracts are dried (Na2SO4)
  3. customthe solvent is evaporated
  4. customThe crude product is purified by silica gel chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-bd342527dbab4b268c90f12665dc57c5
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05552419

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