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Water → HCID 86692457, 화합물

HRID 1748507
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HRID 1748507 반응식
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([C:11]#[N:12])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[Br:23][C:24]1[CH:25]=[CH:26][C:27](F)=[N:28][CH:29]=1.O>O1CCCC1>[Br:23][C:24]1[CH:25]=[CH:26][C:27]([C:8]2([C:11]#[N:12])[CH2:9][CH2:10][C:5]3([O:4][CH2:3][CH2:2][O:1]3)[CH2:6][CH2:7]2)=[N:28][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 2733832Lithium hexamethyldisilazaneHCID 27831685-Bromo-2-fluoropyridineHCID 111164331,4-Dioxaspiro[4.5]decane-8-carbonitrile

생성물 1

HCID 86692457HCID 86692457, 화합물수율 68.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매
2회

실험 절차

After 1,4-dioxaspiro[4,5]decane-8-carbonitrile (2.5 g) was dissolved in tetrahydrofuran (8 ml), 1M tetrahydrofuran-solution of lithium bis(trimethylsilyl)amide (15 ml) was added at 0° C. and stirred for 30 minutes. 5-Bromo-2-fluoropyridine (2.64 g) was further added and stirred at room temperature for two hours. Water was added to the reaction solution, extracted with ethyl acetate and concentrated in vacuo. The residue was purified with silica gel chromatography (n-hexane/ethyl acetate) and the resulting solid was washed with n-hexane to give the titled compound (3.32 g).

후처리

  1. stirringstirred at room temperature for two hours
  2. extractionextracted with ethyl acetate
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified with silica gel chromatography (n-hexane/ethyl acetate)
  5. washthe resulting solid was washed with n-hexane

출처 및 근거

ORD 기록
ord-0c40b9f34c89422fb2684c4ca45a3b4a
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09150555B2

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