Allyl bromide → HCID 67197848, 화합물

HRID 551699노트

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HRID 551699 반응식
[Na].CN([SiH3])[Si](C)(C)C.O1C[CH2:12][CH2:11][CH2:10]1.O1CCCC1.[CH:19]1([CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:22][CH2:21][CH2:20]1.C(Br)C=C>O>[CH:19]1([CH:23]([CH2:12][CH:11]=[CH2:10])[C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:22][CH2:21][CH2:20]1

참가 물질

6

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온도
-78 °C

실험 절차

A 1.9 M tetramethyldisilazane sodium-tetrahydrofuran solution (9.44 mL, 18.0 mmol) was added dropwise over 10 minutes to a tetrahydrofuran (40 mL) solution of ethyl 2-cyclobutylacetate (2.32 g, 16.3 mmol) cooled to −78° C., and the mixture was then stirred at −78° C. for 10 minutes. Subsequently, a tetrahydrofuran (10 mL) solution of allyl bromide (7.90 g, 65.3 mmol) was added dropwise thereto over 10 minutes, and the mixture was stirred at room temperature for 17 hours. The mixture was treated with water, and volatile portions were then removed under reduced pressure. To the obtained liquid, ethyl acetate and water were added, and the obtained organic layer was dried over anhydrous magnesium sulfate. Then, the solvent was distilled off under reduced pressure to obtain the compound of interest as a yellow oil substance (1.80 g, 61%).

후처리

  1. waitover 10 minutes
  2. stirringthe mixture was stirred at room temperature for 17 hours
  3. customwere then removed under reduced pressure
  4. additionTo the obtained liquid, ethyl acetate and water were added
  5. dry with materialthe obtained organic layer was dried over anhydrous magnesium sulfate
  6. distillationThen, the solvent was distilled off under reduced pressure
  7. customto obtain the compound of interest as a yellow oil substance (1.80 g, 61%)

출처 및 근거

ORD 기록
ord-99f6bc43bbdd4fb7b54f431eac15f295
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07947738B2

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