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Ethyl Acetate → HCID 58083500, 화합물

HRID 1254001
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HRID 1254001 반응식
[CH2:1]([N:3]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][C:5]([CH3:12])=[N:4]1)[CH3:2].[I:13]N1C(=O)CCC1=O.CCOC(C)=O>CN(C=O)C.O>[CH2:1]([N:3]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:6]([I:13])[C:5]([CH3:12])=[N:4]1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8857Ethyl AcetateHCID 120273N-IodosuccinimideHCID 22167575Methyl 1-ethyl-3-methyl-1H-pyrazole-5-carboxylate

생성물 1

HCID 58083500HCID 58083500, 화합물수율 47%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매
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실험 절차

To a flask, methyl 1-ethyl-3-methylpyrazol-5-ylcarboxylate (1.00 g, 0.006 mol, Ref. CN1626520A) was dissolved in 10 mL of DMF and N-iodosuccinimide (1.47 g, 0.007 mol) was added in batches. After reacting for 8 h at r.t., the mixture was diluted with 50 mL of water, and then extracted with 50 mL of ethyl acetate. The organic layer was washed with 50 mL of saturated aqueous sodium bicarbonate solution and 50 mL of saturated brine, dried over anhydrous MgSO4 and concentrated under reduced pressure. Column chromatography (EtOAc:P.E.=1:10 as eluent) gave 0.82 g of the title compound as a yellow oil (yield 47%).

후처리

  1. extractionextracted with 50 mL of ethyl acetate
  2. washThe organic layer was washed with 50 mL of saturated aqueous sodium bicarbonate solution and 50 mL of saturated brine
  3. dry with materialdried over anhydrous MgSO4
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-77e9f95127f54d5da99d175609078835
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08455532B2

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