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Water → tert-butyl N-(4-methyl-1-oxopentan-2-yl)carbamate

HRID 2401256
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HRID 2401256 반응식
[OH:1][CH2:2][CH:3]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:4][CH:5]([CH3:7])[CH3:6].I(C1C=CC=CC=1C(O)=O)(=O)=O.O>CS(C)=O>[CH3:6][CH:5]([CH3:7])[CH2:4][CH:3]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:2]=[O:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 1087942-Iodoxybenzoic acidHCID 546110tert-butyl N-(1-hydroxy-4-methylpentan-2-yl)carbamate

생성물 1

HCID 546109tert-butyl N-(4-methyl-1-oxopentan-2-yl)carbamate

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of tert-butyl (1-hydroxy-4-methylpentan-2-yl)carbamate (2.7 g) in DMSO (60 mL) was added 2-iodoxybenzoic acid (3.5 g), and the mixture was stirred at room temperature for 3 hr. Water was added thereto, the resulting insoluble matter was filtered off, and the filtrate was extracted with ethyl acetate. The organic layer was washed with water and brine, and dried over anhydrous magnesium sulfate. After the dessicant was filtered off, the filtrate was concentrated under reduced pressure to afford a crude product of tert-butyl (4-methyl-1-oxopentan-2-yl)carbamate.

후처리

  1. filtrationthe resulting insoluble matter was filtered off
  2. extractionthe filtrate was extracted with ethyl acetate
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationAfter the dessicant was filtered off
  6. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1068b36a8d4649d2b34630d4b93a9902
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08796272B2

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