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Hydrazine → HCID 90373274, Verbindung

HRID 930417
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 930417
[CH3:1][N:2]([CH3:10])/[N:3]=[C:4](\[CH3:9])/[C:5]([F:8])([F:7])[F:6].C([N-]C(C)C)(C)C.[Li+].CCCCCCC.O1CCCC1.C(C1C=CC=CC=1)C.[F:39][CH2:40]/[C:41](=[N:50]/[S@@:51]([C:53]([CH3:56])([CH3:55])[CH3:54])=[O:52])/[C:42]1[CH:47]=[CH:46][CH:45]=[C:44]([CH3:48])[C:43]=1[F:49].C[Al](C)C.NN>C1COCC1.C1(C)C=CC=CC=1>[CH3:1][N:2]([CH3:10])/[N:3]=[C:4](\[C:5]([F:8])([F:7])[F:6])/[CH2:9][C:41]([NH:50][S@@:51]([C:53]([CH3:56])([CH3:55])[CH3:54])=[O:52])([C:42]1[CH:47]=[CH:46][CH:45]=[C:44]([CH3:48])[C:43]=1[F:49])[CH2:40][F:39]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 6

HCID 9321HydrazineHCID 2724682Lithium diisopropylamideHCID 16682925TrimethylaluminumHCID 22742125Tetrahydrofuran heptane ethylbenzolHCID 58668234HCID 58668234, VerbindungHCID 90373039HCID 90373039, Verbindung

Produkt 1

HCID 90373274
HCID 90373274, Verbindung
Ausbeute 180,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of (E)-1,1-dimethyl-2-(1,1,1-trifluoropropan-2-ylidene)hydrazine (2.256 g, 14.63 mmol) in dry THF (20 mL) at −78° C. were added n,n,n′,n′-tetramethylethylenediamine (2.190 ml, 14.63 mmol) and lithium diisopropylamide, 2.0m heptane/tetrahydrofuran/ethylbenzene (7.32 ml, 14.63 mmol) and stirred at this temperature for 30 min. A solution of (R,E)-N-(2-fluoro-1-(2-fluoro-3-methylphenyl)ethylidene)-2-methylpropane-2-sulfinamide (2.0 g, 7.32 mmol) in toluene (12 mL) at −78° C. was treated with trimethylaluminum, 2.0m solution in toluene (3.66 ml, 7.32 mmol) for 10 min and added dropwise to the solution containing the hydrazine at −78° C. The resulting mixture was stirred at this temperature for 1.5 h. The mixture was quenched with saturated NH4Cl, and extracted with EtOAc. The combined organics were dried over Na2SO4, filtered, concentrated and chromatographed on silica gel using 0-50% EtOAc/hexanes to afford a bright yellow oil as (R)-N-((Z)-4-(2,2-dimethylhydrazono)-1,5,5,5-tetrafluoro-2-(2-fluoro-3-methylphenyl)pentan-2-yl)-2-methylpropane-2-sulfinamide (5.66 g, 77% yield, combined). MS m/z=427.9 [M+H]+. Calculated for C18H26F5N3OS: 427.17.

Aufarbeitung

  1. additionadded dropwise to the solution
  2. stirringThe resulting mixture was stirred at this temperature for 1.5 h
  3. customThe mixture was quenched with saturated NH4Cl
  4. extractionextracted with EtOAc
  5. dry with materialThe combined organics were dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customchromatographed on silica gel using 0-50% EtOAc/hexanes

Quellen und Nachweise

ORD-Eintrag
ord-5a57ae2416624dbb997c43a0eb7e0035
Quelldatensatz
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09296734B2

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