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Methanol → HCID 22747784, 화합물

HRID 1641594
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HRID 1641594 반응식
C([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12]([N:14]2[CH2:19][CH2:18][CH:17]([NH:20][S:21]([C:23]([CH3:26])([CH3:25])[CH3:24])=[O:22])[CH2:16][CH2:15]2)=[O:13])=[CH:7][CH:6]=1)(C)(C)C.[CH:27]1[CH:32]=C(C([O-])=O)C(C(O[O-])=O)=[CH:29][CH:28]=1.[Mg+2].C[OH:42]>C(Cl)Cl.O>[CH2:32]([C:5]1[CH:6]=[CH:7][C:8]([NH:11][C:12]([N:14]2[CH2:19][CH2:18][CH:17]([NH:20][S:21]([C:23]([CH3:24])([CH3:25])[CH3:26])(=[O:42])=[O:22])[CH2:16][CH2:15]2)=[O:13])=[CH:9][CH:10]=1)[CH2:27][CH2:28][CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 887MethanolHCID 10130449Monoperoxyphthalic Acid Magnesium SaltHCID 66739112HCID 66739112, 화합물

생성물 1

HCID 22747784HCID 22747784, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

In a mixture of 2 ml of methanol and 2 ml of methylene chloride, 291 mg of 4-t-butylsulfinylaminopiperidine-1-carboxylic acid(4-t-butylphenyl)amide was dissolved. To the mixture, 570 mg of 80%-MMPP (magnesium monoperoxyphthalate hexahydrate) was added and the mixture was stirred at room temperature for 2 hours. The solution was diluted with water and extracted with ethyl acetate. The organic layer was washed with brine and dried over magnesium sulfate anhydride. The solvent was removed under reduced pressure and the residue was purified by silica gel chromatography to give 130 mg of 4-t-butylsulfonylaminopiperidine-1-carboxylic acid(4-butylphenyl)amide (I-120).

후처리

  1. dissolutionwas dissolved
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried over magnesium sulfate anhydride
  5. customThe solvent was removed under reduced pressure
  6. customthe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-35cf59e6d42748dba8317ecb596a1f3b
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08115027B2

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