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

HRID 2387327
Notes
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Reaction equation

HRID 2387327 reaction equation
[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]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

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

Product 1

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

Reagents, catalysts & solvents 1

HCID 8071
1,2-Dimethoxyethane
Solvent

Procedure

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).

Workup

  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

Sources & evidence

ORD record
ord-64d9e1e969e64d82abdd707f6365903a
Source dataset
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08268859B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes