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

HRID 742151
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HRID 742151 반응식
[CH2:1]([N:3]([CH2:7][CH3:8])[C:4]([NH2:6])=[S:5])[CH3:2].Br[CH2:10][C:11](=O)[C:12]([O:14][CH2:15][CH3:16])=[O:13].[O-]S([O-])(=O)=O.[Mg+2]>CC(C)=O>[CH2:1]([N:3]([C:4]1[S:5][CH:10]=[C:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[N:6]=1)[CH2:7][CH3:8])[CH3:2]
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참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 66144Ethyl bromopyruvateHCID 854389Diethylthiourea

생성물 1

HCID 12966399Ethyl 2-(diethylamino)-1,3-thiazole-4-carboxylate수율 140.4%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 0.972 g (7.36 mmol) of N,N-diethylthiourea and 1.02 ml (8.1 mmol) of ethyl bromopyruvate in 25 ml of acetone was treated with excess solid MgSO4 and heated at reflux for 1 h. The resulting mixture was filtered, and concentrated in vacuo. Silica gel chromatography using CHCl3 provided 2.36 g (38%) of the desired compound as an oil. Mass spectrum: (M+H)+ =229.

후처리

  1. temperatureheated
  2. temperatureat reflux for 1 h
  3. filtrationThe resulting mixture was filtered
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a6a6d1634330425a94ede740030650d5
출처 데이터셋
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05552558

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