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Tetrahydrofuran → 2-[(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethoxy]-N-(2,2,3,3,3-pentafluoropropyl)acetamide

HRID 1922623
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1922623
C[Si](C)(C)[N-][Si](C)(C)C.[Na+].O1CCCC1.[Br:16]/[CH:17]=[C:18]1\[CH2:19][CH2:20][CH2:21][C@@:22]2([CH3:30])[C@H:26]\1[CH2:25][CH:24]=[C:23]2[C@@H:27]([OH:29])[CH3:28].Br[CH2:32][C:33]([NH:35][CH2:36][C:37]([F:43])([F:42])[C:38]([F:41])([F:40])[F:39])=[O:34].[Cl-].[NH4+]>CN(C)C=O.CCCCCC>[Br:16]/[CH:17]=[C:18]1\[CH2:19][CH2:20][CH2:21][C@@:22]2([CH3:30])[C@H:26]\1[CH2:25][CH:24]=[C:23]2[C@@H:27]([O:29][CH2:32][C:33]([NH:35][CH2:36][C:37]([F:42])([F:43])[C:38]([F:41])([F:39])[F:40])=[O:34])[CH3:28]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 5

HCID 8028TetrahydrofuranHCID 25517Ammonium ChlorideHCID 2724254Sodium bis(trimethylsilyl)amideHCID 59456520(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethanol2×HCID 594565462-bromo-N-(2,2,3,3,3-pentafluoropropyl)acetamide

Produkt 1

HCID 24746036
2-[(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethoxy]-N-(2,2,3,3,3-pentafluoropropyl)acetamide

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittel2×HCID 8058HexaneLösungsmittel

Reaktionsbedingungen

Temperatur
-15 °C

Versuchsvorschrift

Under a nitrogen atmosphere, a solution of sodium hexamethyldisilazide in tetrahydrofuran (1.1 M, 5.31 ml, 5.84 mmol) was cooled to −15° C., and a solution of (S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethanol (Compound 5: 633.7 mg, 2.337 mmol) in dimethylformamide (1 ml) was added thereto over 4 minutes. The resulting mixture was stirred at −15° C. for 7 minutes, and a solution of 2-bromo-N-(2,2,3,3,3-pentafluoropropyl)acetamide (726 mg, 2.688 mmol) in dimethylformamide (1 ml) was added thereto over 5 minutes. After stirring the reaction solution at −5° C. for 30 minutes, aqueous ammonium chloride solution (5 ml) and hexane (20 ml) were added thereto, and the separation of the solution was conducted. The obtained organic layer was sequentially washed with water (5 ml) and saturated brine (4 ml)/water (1 ml), and the solvent was evaporated. The obtained crude product was purified by silica gel column chromatography to obtain 2-[(S)-1-{(3aS,7E,7aR)-7-(bromomethylene)-3a,4,5,6,7,7a-hexahydro-3a-methyl-1H-indene-3-yl}ethoxy]-N-(2,2,3,3,3-pentafluoropropyl)acetamide (1.08 g, quantitatively).

Aufarbeitung

  1. waitover 5 minutes
  2. stirringAfter stirring the reaction solution at −5° C. for 30 minutes
  3. customthe separation of the solution
  4. washThe obtained organic layer was sequentially washed with water (5 ml) and saturated brine (4 ml)/water (1 ml)
  5. customthe solvent was evaporated
  6. customThe obtained crude product
  7. customwas purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-89a0867db7f64800aea355d36476c984
Quelldatensatz
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08173824B2

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