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Lithium (trimethylsilyl)acetylide → 2-((R)-3-hydroxy-1,1-dimethyl-3-trifluoromethyl-6-trimethylsilanylhex-5-ynyl)benzamide

HRID 2387327
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HRID 2387327 반응식
[CH3:1][C:2]([C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([NH2:16])=[O:15])([CH3:11])[CH2:3][C@:4]1([C:7]([F:10])([F:9])[F:8])[CH2:6][O:5]1.C([Mg]CCCC)CCC.[Li+].[CH3:31][Si:32]([C:35]#[C-:36])([CH3:34])[CH3:33]>COCCOC>[OH:5][C@@:4]([C:7]([F:8])([F:9])[F:10])([CH2:6][C:36]#[C:35][Si:32]([CH3:34])([CH3:33])[CH3:31])[CH2:3][C:2]([C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([NH2:16])=[O:15])([CH3:11])[CH3:1]
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참가 물질

5

반응물 3

HCID 3431600Lithium (trimethylsilyl)acetylideHCID 580261682-[1,1-dimethyl-2-((R)-2-trifluoromethyloxiranyl)ethyl]benzamideHCID 178448196HCID 178448196, 화합물

생성물 1

HCID 580261722-((R)-3-hydroxy-1,1-dimethyl-3-trifluoromethyl-6-trimethylsilanylhex-5-ynyl)benzamide

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

To a stirred, ice-cooled, solution of (trimethylsilyl)acetylene (72.6 mL, 514 mmol) in 500 mL of ethylene glycol dimethyl ether was added n-butyllithium (185 mL of 2.5 M solution in hexanes, 462 mmol). The reaction mixture, which turned from a colorless to a yellowish solution, was stirred for 50 minutes to give a solution of 462 mmol of lithium (trimethylsilyl)acetylide. A stirred solution of 2-[1,1-dimethyl-2-((R)-2-trifluoromethyloxiranyl)ethyl]benzamide (26.5 g, 92.3 mmol) in ethylene glycol dimethyl ether (250 mL) was cooled to −30° C. Dibutylmagnesium (50.8 mL of 1 M solution in heptane, 50.8 mmol) was added and the mixture stirred for 45 minutes. The above solution of lithium (trimethylsilyl)acetylide was added and the stirring continued at −20° C. After 5 minutes, cooling bath was removed and the reaction mixture was stirred for 3 hours and 15 minutes. The reaction was quenched with 600 mL of saturated ammonium chloride solution and extracted with four 250 mL portions of ethyl acetate. The combined organic extracts were washed with two 250 mL portions of brine, dried over anhydrous sodium sulfate, and the solvent removed in vacuo to give 2-((R)-3-hydroxy-1,1-dimethyl-3-trifluoromethyl-6-trimethylsilanylhex-5-ynyl)benzamide as brownish oil (27 g).

후처리

  1. customcontinued at −20° C
  2. waitAfter 5 minutes
  3. temperaturecooling bath
  4. customwas removed
  5. stirringthe reaction mixture was stirred for 3 hours and 15 minutes
  6. customThe reaction was quenched with 600 mL of saturated ammonium chloride solution
  7. extractionextracted with four 250 mL portions of ethyl acetate
  8. washThe combined organic extracts were washed with two 250 mL portions of brine
  9. dry with materialdried over anhydrous sodium sulfate
  10. customthe solvent removed in vacuo

출처 및 근거

ORD 기록
ord-64d9e1e969e64d82abdd707f6365903a
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268859B2

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