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Methyl iodide → HCID 15075812, 화합물

HRID 2073820
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HRID 2073820 반응식
[CH:1](NC(C)C)(C)C.C([Li])CCC.[Li+].CC([N-]C(C)C)C.[F:21][C:22]1[C:27]([Si:28]([CH3:31])([CH3:30])[CH3:29])=[C:26]([F:32])[C:25]([F:33])=[CH:24][C:23]=1[C:34]1[O:35][CH2:36][C:37]([CH3:40])([CH3:39])[N:38]=1.CI>C1COCC1.O>[F:21][C:22]1[C:27]([Si:28]([CH3:31])([CH3:29])[CH3:30])=[C:26]([F:32])[C:25]([F:33])=[C:24]([CH3:1])[C:23]=1[C:34]1[O:35][CH2:36][C:37]([CH3:40])([CH3:39])[N:38]=1
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참가 물질

8

반응물 5

HCID 6328Methyl iodideHCID 7912DiisopropylamineHCID 2724682Lithium diisopropylamideHCID 14774099HCID 14774099, 화합물HCID 178418339Butyllithium

생성물 1

HCID 15075812HCID 15075812, 화합물수율 90.6%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

A solution of 0.64 ml (4.57 mmol) of diisopropylamine in 20 ml of dry THF under argon was cooled to -78° C. and treated with 2.1 ml (4.20 mmol) of 2.0N n-butyllithium. The LDA solution was stirred at -78° C. for 15 minutes, then warmed to 0° C. To this solution was added a solution of 1.05 g (3.5 mmol) of 2-(2,4,5-trifluoro-3-trimethylsilylphenyl)-4,4-dimethyl-2-oxazoline in 5 ml of THF; the reaction mixture was stirred at 0° C. for 45 minutes, then quenched with 1.50 g (10.6 mmol) of methyl iodide. The solution was stirred at room temperature for three hours and diluted with water. The organic layer was washed with water, dried over magnesium sulfate, and concentrated to give 1.00 g of the title compound as an oil.

후처리

  1. stirringThe solution was stirred at room temperature for three hours
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-b0ffcb1cdb264f7281bc9a7ad7c95400
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04920120

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