Sodium hydride → HCID 66588098, Verbindung

HRID 625227

Reaktionsgleichung

Reaktionsgleichung von HRID 625227
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][OH:7].[H-].[Na+].Cl[C:16]1[CH:21]=[C:20]([C:22]2[CH:27]=[C:26]([N:28]3[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)[CH:25]=[CH:24][C:23]=2[N+:34]([O-:36])=[O:35])[N:19]=[CH:18][N:17]=1>CN(C=O)C>[N+:34]([C:23]1[CH:24]=[CH:25][C:26]([N:28]2[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33]2)=[CH:27][C:22]=1[C:20]1[CH:21]=[C:16]([O:7][CH2:6][C:5]2[CH:8]=[CH:9][CH:10]=[C:3]([C:2]([F:11])([F:12])[F:1])[CH:4]=2)[N:17]=[CH:18][N:19]=1)([O-:36])=[O:35]

Komponenten

5

Edukt 3

HCID 24758Sodium hydrideHCID 676813-(Trifluoromethyl)benzylic alcoholHCID 86705928HCID 86705928, Verbindung

Produkt 1

HCID 66588098HCID 66588098, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 99 mg of 3-(trifluoromethyl)benzyl alcohol in 2 mL of DMF was added 27 mg of a 50% dispersion of sodium hydride in oil. After 15 min the solution was treated with 150 mg of intermediate 3.1b. After an additional 2 h the reaction mixture was partitioned between water and ethyl acetate. The organic extracts were washed with brine and dried (Na2SO4). The solvent was evaporated to give a yellow syrup that was used directly in the next step.

Aufarbeitung

  1. customAfter an additional 2 h the reaction mixture was partitioned between water and ethyl acetate
  2. washThe organic extracts were washed with brine
  3. dry with materialdried (Na2SO4)
  4. customThe solvent was evaporated
  5. customto give a yellow syrup that

Quellen und Nachweise

ORD-Eintrag
ord-4969a3e7c00549bbbf2591705a6162b3
Quelldatensatz
uspto-grants-2016_04
Patentnummer
US09301951B2

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