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Water → HCID 66599153, 화합물

HRID 1038596
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HRID 1038596 반응식
[O:1]1[C:10]2[C:5](=[N+:6]([O-])[CH:7]=[CH:8][CH:9]=2)[O:4][CH2:3][CH2:2]1.[CH2:12]([N:14](CC)CC)C.O>C(#N)C>[O:1]1[C:10]2[C:5](=[N:6][C:7]([C:12]#[N:14])=[CH:8][CH:9]=2)[O:4][CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 8471TriethylamineHCID 66598282HCID 66598282, 화합물

생성물 1

HCID 66599153HCID 66599153, 화합물수율 97.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
100 °C

실험 절차

Under an argon atmosphere, 2,3-dihydro-[1,4]dioxino[2,3-b]pyridine 5-oxide (102 mg, 666 μmol) was dissolved in actonitrile (700 μL), added triethylamine (202 mg, 2.00 mmol) and trimethylsilylnitrile (529 mg, 5.33 mmol) at room temperature, and the mixture was stirred at 100° C. overnight. Under ice-cold conditions, water was added, and the reaction solution was extracted with ethyl acetate, washed with brine, dried over anhydrous sodium sulfate, and concentrated in vacuo. The obtained residue was purified by silica-gel column chromatography (chloroform/methanol), and the title compound (105 mg (yield 97%)) was obtained as a brown solid.

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후처리

  1. extractionthe reaction solution was extracted with ethyl acetate
  2. washwashed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe obtained residue was purified by silica-gel column chromatography (chloroform/methanol)

출처 및 근거

ORD 기록
ord-0fc86d2f167d4647a16c9727f9eadb45
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08551985B2

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