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Sulfuric acid magnesium salt (1:1) → Ethyl 2-(methoxymethyl)-1,3-thiazole-4-carboxylate

HRID 1174127
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HRID 1174127 반응식
[CH3:1][O:2][CH2:3][C:4](=[S:6])[NH2:5].Br[CH2:8][C:9](=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11].S([O-])([O-])(=O)=O.[Mg+2]>CC(C)=O>[CH3:1][O:2][CH2:3][C:4]1[S:6][CH:8]=[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[N:5]=1
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참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 66144Ethyl bromopyruvateHCID 203233692-Methoxyethanethioamide

생성물 1

HCID 45117589Ethyl 2-(methoxymethyl)-1,3-thiazole-4-carboxylate수율 57%

시약·촉매·용매 1

HCID 180Acetone용매

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온도
25 °C

실험 절차

A solution containing the product from Example 6B (7 g, 66.6 mmol) in acetone (270 mL) was treated with ethyl bromopyruvate (8.4 mL, 66.6 mmol) and magnesium sulfate (7.9 g, 66.6 mmol), heated at reflux for 16 hours, cooled to 25° C., filtered and concentrated. The residue was chromatographed on silica gel eluting with chloroform to give the title compound (7.6 g, 57% yield).

후처리

  1. temperatureheated
  2. temperatureat reflux for 16 hours
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was chromatographed on silica gel eluting with chloroform

출처 및 근거

ORD 기록
ord-c309c551cafd42dfad164da8f90a272b
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07834043B2

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