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Ethanol → methyl-(2E)-3-methyl-5-[(1-phenyl-1-H-tetrazol-5-yl)thio]pent-2-enoate

HRID 1160584
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HRID 1160584 반응식
OO.C(O)C.[CH2:6]([O:8][C:9](=[O:27])/[CH:10]=[C:11](\[CH3:26])/[CH2:12][CH2:13][S:14][C:15]1[N:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:18]=[N:17][N:16]=1)C>C(OCC)(=O)C>[CH3:6][O:8][C:9](=[O:27])/[CH:10]=[C:11](\[CH3:26])/[CH2:12][CH2:13][S:14][C:15]1[N:19]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[N:18]=[N:17][N:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 784Hydrogen PeroxideHCID 59516418ethyl-(2E)-3-methyl-5-[(1-phenyl-1-H-tetrazol-5-yl)thio]pent-2-enoate

생성물 1

HCID 59516421methyl-(2E)-3-methyl-5-[(1-phenyl-1-H-tetrazol-5-yl)thio]pent-2-enoate수율 99.4%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

About 30% hydrogen peroxide solution (47.4 ml, 418.0 mmol) solution of hexaammonium heptamolybdate tetrahydrate (542 mg, 0.44 mmol) was added to an ethanol (200 ml) solution of ethyl-(2E)-3-methyl-5-[(1-phenyl-1-H-tetrazol-5-yl)thio]pent-2-enoate (13.31 g, 41.80 mmol) at room temperature. After stirred for at the same temperature for 12 hours, the reaction solution was diluted with ethyl acetate and washed with distilled water and brine. After the organic layer was dried over anhydrous sodium sulfate and the drying agent was filtered off, the organic layer was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography (Merck, commercial name Silica Gel 60, 230-400 mesh; hexane:ethyl acetate=4:1) to obtain the title compound (12.65 g) as a white solid.

후처리

  1. washwashed with distilled water and brine
  2. dry with materialAfter the organic layer was dried over anhydrous sodium sulfate
  3. filtrationthe drying agent was filtered off
  4. concentrationthe organic layer was concentrated under reduced pressure
  5. customThe obtained residue was purified by silica gel column chromatography (Merck, commercial name Silica Gel 60, 230-400 mesh; hexane:ethyl acetate=4:1)

출처 및 근거

ORD 기록
ord-954b3139024747e8adb832e3ddc5be8f
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07816401B2

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