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Diethyl Ether → 1-(4-Methyl-1,2,3-thiadiazol-5-yl)ethan-1-one

HRID 396537
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HRID 396537 반응식
CON(C)[C:4]([C:6]1[S:10][N:9]=[N:8][C:7]=1[CH3:11])=[O:5].[CH2:13](OCC)C.C[Mg]I>C1COCC1>[C:4]([C:6]1[S:10][N:9]=[N:8][C:7]=1[CH3:11])(=[O:5])[CH3:13]
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참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 23003463HCID 23003463, 화합물HCID 178418373HCID 178418373, 화합물

생성물 1

HCID 230035181-(4-Methyl-1,2,3-thiadiazol-5-yl)ethan-1-one수율 87%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of N-methoxy-N-methyl-4-methyl-1,2,3-thiadiazole-5-carboxamide (11.31 g, 60.4 mmol) in THF (100 ml) was added 2M diethyl ether solution of methylmagnesium iodide (45.3 ml, 90.6 mmol) over 0.5 h at 0° C. The mixture was allowed to warm to room temperature and stirred for 3 h. The mixture was quenched with saturated aqueous ammonium chloride (100 ml) and then extracted with diethyl ether (200 ml×2). The extracts were dried (MgSO4) and concentrated to give 7.49 g (87%) of the title compound as a pale brown oil.

후처리

  1. customThe mixture was quenched with saturated aqueous ammonium chloride (100 ml)
  2. extractionextracted with diethyl ether (200 ml×2)
  3. dry with materialThe extracts were dried (MgSO4)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8c8839183b754a71ad88b973b7d40d88
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06608070B1

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