Hexane → 5,5,5-Trifluoro-1-pentynyl-tri(n-butyl)stannane

HRID 412161노트

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HRID 412161 반응식
Br[C:2](Br)=[CH:3][CH2:4][CH2:5][C:6]([F:9])([F:8])[F:7].[Li]CCCC.[CH2:16]([Sn:20](Cl)([CH2:25][CH2:26][CH2:27][CH3:28])[CH2:21][CH2:22][CH2:23][CH3:24])[CH2:17][CH2:18][CH3:19].CCCCCC>O1CCCC1>[F:7][C:6]([F:9])([F:8])[CH2:5][CH2:4][C:3]#[C:2][Sn:20]([CH2:21][CH2:22][CH2:23][CH3:24])([CH2:25][CH2:26][CH2:27][CH3:28])[CH2:16][CH2:17][CH2:18][CH3:19]

참가 물질

6

반응물 4

HCID 8058HexaneHCID 15096Tributyltin ChlorideHCID 185361221,1-Dibromo-5,5,5-trifluoro-1-penteneHCID 178418339Butyllithium

생성물 1

HCID 185360835,5,5-Trifluoro-1-pentynyl-tri(n-butyl)stannane

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

To a −78° C. solution the product from Step A (0.935 mg, 3.31 mmol) in 10 mL of tetrahydrofuran was added n-BuLi solution (2.65 mL, 6.63 mmol, 2.5 M hexanes) dropwise. The reaction was stirred at −78° C. for one hour, then allowed to warm to room temperature for one hour. The solution was cooled to 0° C., and tributyltin chloride (0.898 mL, 3.31 mmol) was added. After 10 minutes, the solution was poured into hexane, washed with saturated NaHCO3 solution and brine, dried (Na2SO4), filtered, and concentrated in vacuo. The product was isolated as a brown liquid which was used without further purification.

후처리

  1. temperatureto warm to room temperature for one hour
  2. temperatureThe solution was cooled to 0° C.
  3. waitAfter 10 minutes
  4. washwashed with saturated NaHCO3 solution and brine
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe product was isolated as a brown liquid which
  9. customwas used without further purification

출처 및 근거

ORD 기록
ord-4da94bd174aa4d6ab284c7a2bec94def
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06562823B1

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