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Aluminum(III) Chloride → 1-Methyl-2-sulfanylidene-6-(trifluoromethyl)-2,3-dihydropyrimidin-4(1H)-one

HRID 584558
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HRID 584558 반응식
[CH3:1][N:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5](=[O:12])[N:4](CC2C=CC=CC=2)[C:3]1=[S:20].[Cl-].[Al+3].[Cl-].[Cl-]>C1(C)C=CC=C(C)C=1>[CH3:1][N:2]1[C:7]([C:8]([F:10])([F:11])[F:9])=[CH:6][C:5](=[O:12])[NH:4][C:3]1=[S:20]
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참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 223409922,3-Dihydro-1-methyl-3-(phenylmethyl)-2-thioxo-6-(trifluoromethyl)-4(1H)-pynmidinone

생성물 1

HCID 223409891-Methyl-2-sulfanylidene-6-(trifluoromethyl)-2,3-dihydropyrimidin-4(1H)-one수율 48.6%

시약·촉매·용매 1

HCID 7929M-Xylene용매

실험 절차

2,3-Dihydro-1-methyl-3-(phenylmethyl)-2-thioxo-6-(trifluoromethyl)-4(1H)-pyrimidinone (1.0 g) was dissolved in m-xylene (15 ml) and anhydrous aluminum chloride (0.58 g) was added. The solution was refluxed for 4 hr and poured onto ice water. Extraction with ethyl acetate and evaporation of the solvent in vacuo afforded a residue which was triturated with diethyl ether to afford the title compound (0.34 g). 1H NMR, CDCl3, 3.86 (3H, m), 6.49 (1H, s), 10.62 (1H, br s).

후처리

  1. temperatureThe solution was refluxed for 4 hr
  2. additionpoured onto ice water
  3. extractionExtraction
  4. customwith ethyl acetate and evaporation of the solvent in vacuo
  5. customafforded a residue which
  6. customwas triturated with diethyl ether

출처 및 근거

ORD 기록
ord-3cc6b55465fd4df593b937d09512ff0d
출처 데이터셋
uspto-grants-2005_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06927193B2

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